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Production method for oxazine resin

A technology of oxazine resin and paraformaldehyde, which is applied in the field of preparation of oxazine resin, can solve the problems of low resin cyclization rate, achieve the effects of low production cost, simple and stable preparation method, and stable reaction

Inactive Publication Date: 2008-07-16
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the resin obtained by the catalytic reaction in the solvent, the ring formation rate is lower

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Example 1: 270 grams (3 mol) of aniline, 342 grams (3.0 mol phenolic hydroxyl) of bisphenol A, and 180 grams (6 mol) of paraformaldehyde were stirred and mixed uniformly in a beaker at room temperature. Pour 1 / 10 of the mixture into a 1000 ml flask. When the temperature of the heating flask was raised to 70°C, the reaction was violent. After about 5 minutes, the second batch of 1 / 10 mixture was added after the reaction was stable. The remaining mixture was added sequentially. After the raw materials are added, the reaction temperature is maintained at 110° C., and the reaction is carried out for 10-15 minutes in a state of reflux with a small amount of water. Then, the reflux device was removed and the water was evaporated instead. Water was distilled off at 130°C. After half an hour, discharge the material in a stainless steel pan while it is hot to obtain a kind of oxazine resin. The resin yield is 95%, the resin softening point is 73°C, and the ring-forming rate ...

Embodiment 2

[0014] Example 2: 270 grams (3mol) of aniline, 342 grams (3.0mol phenolic hydroxyl) of bisphenol A, and 180 grams (6mol) of paraformaldehyde were stirred and mixed in a dropping funnel at room temperature, kept stirring, and put 1 / 10 The mixture was placed in a 1000 ml flask. When the heating flask was heated to 60°C, the reaction was violent, and after 10 minutes, the reaction tended to be stable. Start adding the mixture dropwise. Control the rate of addition within one hour. Since the mixture is a mixture of solid and liquid, it must be fully stirred during the dropping process and keep the dropping valve unblocked and free of aggregates. After the raw materials are added, the reaction temperature is maintained at 100-110° C., and the reaction is carried out for 60 minutes under the reflux state of a small amount of water. Then, the reflux device was removed and the water was evaporated instead. Water was distilled off at 110°C. Discharge the material in a stainless s...

Embodiment 3

[0015] Example 3: 270 grams (3mol) of aniline, 282.3 grams (3mol) of phenol, and 180 grams (6mol) of paraformaldehyde were stirred and mixed in the dropping funnel at room temperature, and kept stirring, and put 1 / 10 mixture in 1000 ml flask. When the temperature of the heating flask was raised to 130°C, the reaction was violent. After 8 minutes, the second batch of 1 / 10 mixture was added after the reaction was stable. The remaining mixture was added sequentially. After the raw materials are added, the reaction temperature is maintained at 100-110° C., and the reaction is carried out for 10 minutes under the reflux state of a small amount of water. Then, the reflux device was removed and the water was evaporated instead. Distill water at 130-135°C. Discharge the material in a stainless steel pan while it is hot to obtain an oxazine resin. The yield of the resin is 94%, and the softening point of the resin is 76°C.

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Abstract

The invention provides a method used for preparing oxaxine resin, which comprises steps that: primary amine, hydroxybenzene and paraform are mixed at a temperature lower than 40 DEG C with the mol ratio of 1:1:2; the mixture are added into a reactor for reacting at 50-130 DEG C batch by batch, with 5-10 minutes reaction for each batch; or the mixture is continuously added into the 50-130 DEG C reactor for reacting, the adding of which is finished within 60-120 minutes; then the temperature is raised to 110-140 DEG C to vaporize moisture produced by the reaction; the oxaxine resin is obtained after the discharging of material. The preparation method of the invention is simple and stable, the reaction is stably carried out in standard atmosphere without a catalyzer and the byproduct of is water without pollution. The preparation method has low requirement on devices, with low manufacturing cost, thereby being easy to realize industrialized production.

Description

technical field [0001] The invention belongs to the field of polymer synthetic materials, and in particular relates to a preparation method of oxazine resin. Background technique [0002] Benzoxazine resin has high heat resistance and non-combustibility, and can be used as composite material resin matrix, insulating paint, potting compound, etc., and has broad application prospects in aerospace, aviation, navigation and other fields. Patent CN 1884376A, "Heat-resistant benzoxazine resin compound and its preparation method and application" is to mix 50-95 parts by weight of benzoxazine resin intermediate, liquid resin or solid powder of aromatic compound containing aldehyde group 0-50 parts by weight and / or 50-0 parts by weight of an aldehyde-containing benzoxazine resin intermediate, dissolved in a solvent at room temperature-50°C to obtain a heat-resistant benzoxazine resin composite solution, and then the The solution adopts the coating or impregnation process to prepare ...

Claims

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Application Information

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IPC IPC(8): C08G73/06
Inventor 林晓丹
Owner SOUTH CHINA UNIV OF TECH