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Preparation method of benzoxazine compound

A technology of benzoxazine and compounds, which is applied in the field of preparation of benzoxazine compounds, can solve the problems of low product yield and low purity, reduce adverse effects, facilitate the process, and reduce the cost and complexity of the process Effect

Active Publication Date: 2015-02-18
SUZHOU TAIHU ELECTRIC ADVANCED MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since the suspension method uses water as the dispersion medium, the production cost is reduced and the environmental pollution caused by the solvent is avoided. However, the product synthesized by this method has a low yield and low purity, and subsequent treatment is required.

Method used

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  • Preparation method of benzoxazine compound
  • Preparation method of benzoxazine compound
  • Preparation method of benzoxazine compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Place a 1000 ml four-neck flask with a thermometer and stirring in an ice-water bath at 4°C, add 400 grams of water, 23.5 grams (0.253 mol) of aniline, and 5 grams of toluene, start stirring, and then slowly drop it with a constant pressure drop funnel. Add 45 grams (0.555 mol) of 37 wt% formaldehyde solution, stir for about 5 hours, then add 28.5 grams (0.125 mol) of bisphenol A, heat up to 85 ° C, keep warm for 5 hours, pour out the reactant after the water becomes clear, and obtain After the product is cooled, it forms a light yellow sulfur block, which is bisphenol A benzoxazine.

[0033] The infrared test was carried out on the obtained product. The manufacturer of the FTIR instrument was BRUKER, model TENSOR 27. The resulting infrared spectrum can be found in figure 1 . see figure 1 , of which 946cm ‐1 It is the characteristic peak of oxazine ring, 3000cm ‐1 The nearby peak is the characteristic peak of C‐H stretching vibration on the benzene ring, 1601cm ‐1...

Embodiment 2

[0035] Place a 1000 ml four-necked flask with a thermometer and stirring in a hot water bath at 35°C, add 400 grams of water, 23.5 grams of aniline, and 5 grams of toluene, start stirring, and then slowly add 37wt% 45 grams of formaldehyde aqueous solution, stirred for about 3 hours, then added 28.5 grams of bisphenol A, raised the temperature to 85 ° C, and kept it warm for 5 hours. After the water became clear and transparent, poured out the reactant, and the obtained product formed a light yellow sulfur block after cooling. (the color is slightly darker than the color of the product of Example 1), that is, bisphenol A benzoxazine.

Embodiment 3

[0037] Place a 1000 ml four-neck flask with a thermometer and stirring in an ice-water bath at 4°C, add 400 grams of water, 23.5 grams of aniline, and 5 grams of toluene, start stirring, and then slowly add 37 wt% formaldehyde dropwise with a constant pressure drop funnel 45 grams of aqueous solution, stirred for about 3 hours, then added 28.5 grams of bisphenol A, raised the temperature to 80°C, and kept the temperature for 7 hours. After the water became clear and transparent, the reaction product was poured out. That is bisphenol A benzoxazine.

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Abstract

The invention relates to a preparation method of a benzoxazine compound. The preparation method comprises the following steps: adding water, an amine compound and a solvent into a reactor, stirring, dripping an aqueous formaldehyde solution, stirring for 2-5 hours, adding a phenolic compound, heating up to 55-100 DEG C, ending reaction when water in a system becomes clear and transparent, and cooling an obtained product to form a cake, namely the benzoxazine compound, wherein the adding mass of the solvent is 5-40% of that of the benzoxazine compound. In the preparation method, the advantages of body melt polymerization and suspension polymerization are combined, and a small amount of solvent is used for substituting a suspending agent, so that the preparation method has the advantages of high yield of the body melt polymerization, easiness in heat control of the suspension polymerization, and easiness in reactant mixing in a solution method; a complicated process of cleaning and purifying for removing the solvent in the solution method, and a subsequent processing requirement for removing the suspending agent in a suspension method can be avoided; the product obtained by the preparation method has the higher purity and better heat resistance than those of a product obtained in the solution method.

Description

technical field [0001] The invention relates to a preparation method of a benzoxazine compound. Background technique [0002] According to statistics, in 2011, the motor holding capacity in my country was 1.7 billion kilowatts, accounting for 64% of the total electricity consumption of the whole society, and 75% of the electricity consumption in the industrial field was in the motor. According to calculations, every one percentage point increase in motor efficiency can save more than 26 billion kilowatt-hours of electricity every year. In the field of high-voltage motors, improving the performance of insulating materials mainly includes improving heat resistance, reducing energy consumption and environmental pollution of insulating materials. [0003] Benzoxazine is a new type of phenolic resin, a nitrogen-containing six-membered ring heterocyclic compound obtained by the reaction of phenolic compounds, formaldehyde, and primary amine compounds. It retains some advantages ...

Claims

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Application Information

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IPC IPC(8): C07D265/16
CPCC07D265/16
Inventor 王世强景录如吴斌井丰喜程新建黄芬屈永明
Owner SUZHOU TAIHU ELECTRIC ADVANCED MATERIAL CO LTD
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