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Method for preparing aminophenol triglycidyl group compound

A technology of triglycidol and aminophenol, applied in the direction of organic chemistry, can solve the problems of shortening reaction time and increasing cost, and achieve the effect of shortening reaction time

Active Publication Date: 2008-03-12
SHANGHAI PLASTICS RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Judging from the current situation, the use of catalysts to shorten the reaction time is indeed an advantage. As for the elimination of by-products, we still need to continue to work hard. From the perspective of process production, the use of catalysts also increases the cost accordingly.

Method used

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  • Method for preparing aminophenol triglycidyl group compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Put 1203g (13 moles) of epichlorohydrin and 552g of ethylene glycol, blown nitrogen, stirred and added 109g (1 mole) of p-aminophenol in batches at 40°C, controlled to complete the addition within 2.5 hours, and kept the temperature for 4 hours when the temperature rose to 50°C. Then, 320 g (4 moles of NaOH) of 50% by weight sodium hydroxide aqueous solution was added dropwise, and added dropwise into the reaction system three times, and reacted at 55° C. for 3 hours after the dropwise addition was completed. Followed by vacuum distillation, recovery of epichlorohydrin, distillation at 60°C / 600mmHg until there is almost no distillate. The distillate was allowed to stand overnight and separated into layers, epichlorohydrin was circulated as the raw material for the reaction, the mixture of water and ethylene glycol was excluded, and another treatment was performed. After epichlorohydrin was distilled under reduced pressure, the residue was extracted with 1200ml of tolue...

Embodiment 2

[0019] In addition to replacing p-aminophenol with m-aminophenol, and replacing ethylene glycol with ethanol, the amount of epichlorohydrin added is 1388g (15 moles), the feeding temperature is 25°C, the feeding time is 3 hours, and the temperature is kept at 55°C for 5 hours. After the alkali is finished, react at 60° C. for 3 hours, distill out epichlorohydrin at a temperature of 65° C., and a pressure of 500 mmHg. Other formulations and operating steps are exactly the same as in Example 1. As a result, a yellow-brown m-aminophenol triglycidyl compound was obtained, with a yield of 263 g, a yield of 95%, an epoxy value of 0.85, a viscosity of 2490 mPa.S, and a Gardner hue of 5.

Embodiment 3

[0021] In addition to replacing p-aminophenol with o-aminophenol and isopropanol instead of ethylene glycol, the amount of epichlorohydrin added is 833g (9 moles), the feeding temperature is 55°C, the feeding time is 2 hours, and it is kept at 45°C for 3 hours. Hour, other formula and operating procedure are exactly the same as embodiment 1, the result obtains yellow-brown o-aminophenol triglycidyl compound, and its yield is 269g, yield 97%, epoxy value 1.00, viscosity 2485mPa.S, Gardner hue is 7.

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Abstract

A preparation method of the aminophenol tri-glycidyl compound comprises: the molar ratio between the aminophenol and the epichlorohydrin is 1 to between 9 and 15; at the temperature between 25 and 55 DEG C, the aminophenol is added into the mixture of the epichlorohydrin and alcohol solvent in patches; the material feeding time is 2 to 3 hours; the temperature between 45 and 55 DEG C is maintained for 3 to 5 hours; then the aqueous solution of sodium hydroxide of 50 percent of the weight ratio is added; the molar ratio between the added sodium hydroxide and the aminophenol is 4 to 1; and the aqueous solution of sodium hydroxide is added in three times; the reaction is done for 3 hours at the temperature between 50 and 60 DEG C; the excessive epichlorohydrin and alcohol solvent are vaporized; the solution is statically laid to be separated; the distilled solution of the epichlorohydrin is recycled to be used as the raw material of the reaction. The residue in the reactor is extracted with toluene and is washed with water for 3 times; the left toluene product is vaporized; the color of the product is yellow brown; the collection rate is between 95 and 98 percent; the epoxy value is between 0.85 and 1.00; the viscosity is less than or equal to 2500mPa.S; the hue of the added sodium is between 5 and 7.

Description

1. Technical field [0001] The present invention relates to the preparation method of trifunctional epoxy resin, relate to the preparation method of aminophenol triglycidyl compound more precisely. 2. Background technology [0002] The chemical structure of the aminophenol triglycidyl compound of the present invention is: [0003] [0004] As far as its precursor aminophenol is concerned, the amino group can be in the para-, meta-, ortho-position of the phenolic hydroxyl group. [0005] Due to the low viscosity of aminophenol triglycidyl compounds, excellent storage stability, glass transition temperature of cured molded parts as high as 230°C, coupled with excellent workability and heat resistance, this product is widely used as electrical insulation materials, laminated products, Adhesives and structural materials, etc. For example: JP.03-21631, 1991-01-30 disclosed carbon fiber composite materials made of aminophenol triglycidyl compounds. US Pat.No6,468,659.oct.22, ...

Claims

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Application Information

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IPC IPC(8): C07D303/36
Inventor 李伟烘单美成吴功柏朱丽君
Owner SHANGHAI PLASTICS RES INST CO LTD
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