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Method for producing benzoxazine resin

A technology of benzoxazine and its manufacturing method, which is applied in the field of manufacturing benzoxazine resin, and can solve problems such as laborious waste, lack of solubility, inability to stir, etc.

Inactive Publication Date: 2004-05-12
HITACHI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because benzoxazine resin has no solubility and affinity for water, the viscosity of the reaction solution increases at this time, and it cannot be stirred, and the disposal work is also very troublesome.

Method used

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  • Method for producing benzoxazine resin

Examples

Experimental program
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Effect test

Embodiment 1

[0034]In a 5-liter flask equipped with a thermometer, a stirrer, a cooling tube, and a drop-in device, it is 1040 grams of phenol novolac resin and 1,040 grams of 400 phenol novolac resins that the number average molecular weight (utilizing gel permeation chromatography, using a standard polystyrene calibration curve to measure) is 400. 560 grams of ketones are stirred and dissolved, and then 600 grams of paraformaldehyde are added thereto. While stirring, 931 grams of aniline was added dropwise for 1 hour. At this time, the temperature of the reaction solution was 81°C. Thereafter, the reaction was carried out under reflux (80-82° C.) for 7 hours, and then, under the conditions of heating and 360 mm Hg, concentration under reduced pressure was started. Continue to concentrate while maintaining the reduced pressure, and increase the reduced pressure to 90 mmHg when the temperature of the reaction solution reaches 110°C. When it was confirmed that there was no more effluent (...

Embodiment 2

[0036] Add 140 grams of bisphenol A1 and 900 grams of butanone in a 5-liter flask equipped with a thermometer, a stirrer, a cooling pipe, and a dripping device, stir and dissolve, and add 1622 grams of 37% formalin solution to it, while stirring, 931 grams of aniline were added dropwise in 1 hour. At this time, the temperature of the reaction solution was 81°C. Then, it reacted for 7 hours under reflux (80-82 degreeC). Then, under the conditions of heating and 360 mm Hg, start to carry out concentration under reduced pressure. Continue to concentrate while maintaining the reduced pressure, and increase the reduced pressure to 90 mmHg when the temperature of the reaction solution reaches 85°C. When it was confirmed that there was no more effluent (at this time, the melting temperature of the resin was 100° C.), the resin was taken out and placed on a tray.

[0037] The obtained resin had a softening point of 75°C and a melt viscosity of 2.5 poise (125°C). The temperature of...

Embodiment 3

[0039] Add 1140 grams of bisphenol A1 and 920 grams of methanol into a 5-liter flask equipped with a thermometer, a stirrer, a cooling tube, and a dripping device, and stir to dissolve. Then add paraformaldehyde 652 grams wherein. While stirring, 930 g of aniline was added dropwise for 1 hour. At this time, the temperature of the reaction solution was 79°C. Then, it reacted for 7 hours under reflux (78-80 degreeC). Then, under the conditions of heating and 360 mm Hg, start to concentrate under reduced pressure. Continue to concentrate while maintaining the reduced pressure, and increase the reduced pressure to 90 mmHg when the temperature of the reaction solution reaches 85°C. When it was confirmed that there was no more effluent (at this time, the melting temperature of the resin was 100° C.), the resin was taken out and placed on a tray. The softening point of the resin was 76°C, and the melt viscosity at 125°C was 2.7 poise. At the minimum point (R), the temperature of...

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Abstract

The present invention discloses a process for producing a benzoxazine resin which comprises the steps of reacting a phenol compound, an aldehyde compound and a primary amine in the presence of an organic solvent to synthesize a benzoxazine resin and removing generated condensation water and the organic solvent from a system under heating and a reduced pressure, wherein a pressure in the reaction system at the time of removal is set to 260 mmHg or higher.

Description

technical field [0001] The present invention relates to a method for producing a benzoxazine resin having an oxazine ring. Background technique [0002] Regarding the synthesis of benzoxazine resins, it is published in Journal of Organic Chemistry (J.Org.Chem) volume 30, page 3423 (1965) (author: Burke), JP-A 60-155234, JP-A Gazette No. 60-177074, JP-A-49-47378, Journal of Polymer Science Part A: Polymer Chemistry (J.Polym.Sci.PartA: Polym.Chem.) Vol. 32, p. 1121 (1994) (Author : Ishida, etc.), etc., according to these documents, as a synthesis method of benzoxazine resin, it is described (1) a method of adding formaldehyde to a mixed solution of a compound having a phenolic hydroxyl group and a primary amine; A method of adding a phenolic hydroxyl group to a reacted solution of a primary amine and formaldehyde, (3) After the synthesis is carried out by adding a mixture of a primary amine and a phenolic hydroxyl group to formaldehyde, the reaction solvent and the generated ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G14/06C08G14/073
CPCC08G14/06
Inventor 相沢辉树平井康之沼田俊一
Owner HITACHI CHEM CO LTD
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