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Method for preparing aminophenol triglycidyl group compound

A technology of triglycidyl and aminophenol, applied in directions such as organic chemistry, can solve the problems such as shortening the reaction time and increasing the cost, and achieve the effect of shortening the reaction time

Active Publication Date: 2010-07-28
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] A 5-liter four-necked flask equipped with a stirrer, a thermometer, a nitrogen introduction tube, a dropping funnel, and a condensation separator of an azeotropic mixture of epichlorohydrin and water was filled with 1203g (13 moles) of epichlorohydrin and 552g of ethylene glycol, vented with nitrogen, stirred at 40°C and added 109g (1 mole) of p-aminophenol in batches, controlled to complete the addition within 2.5 hours, and kept the temperature at 50°C for 4 hours. Then, 320 g (4 mol NaOH) of 50% by weight sodium hydroxide aqueous solution was added dropwise, and then added dropwise to the reaction system three times, and reacted at 55° C. for 3 hours after the addition was completed. Followed by vacuum distillation, recovery of epichlorohydrin, and distillation at 60°C / 600mmHg until there is almost no distillate. The distillate is allowed to stand overnight, layered, and epichlorohydrin is recycled as raw material for the reaction. The mixture of water and ethylene gl...

Embodiment 2

[0019] In addition to using meta-aminophenol instead of p-aminophenol and ethanol instead of ethylene glycol, 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 completed, the reaction is carried out at 60°C for 3 hours, and the epichlorohydrin is distilled out at a temperature of 65°C and a pressure of 500mmHg. The other formulas and operation steps are exactly the same as those in Example 1. As a result, a yellow-brown m-aminophenol triglycidyl compound was obtained. The yield was 263 g, the yield was 95%, the epoxy value was 0.85, the viscosity was 2490 mPa.S, and the Gardner hue was 5.

Embodiment 3

[0021] In addition to using o-aminophenol instead of p-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 the temperature is kept at 45°C 3 Hours, other formulas and operating steps are exactly the same as in Example 1. As a result, a yellow-brown o-aminophenol triglycidyl compound is obtained. The yield is 269g, the yield is 97%, the epoxy value is 1.00, and the viscosity is 2485mPa.S. The hue of Gardner 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 a method for preparing trifunctional epoxy resins, more specifically, to a method for preparing aminophenol triglycidyl compounds. 2. Background technology [0002] The chemical structure of the aminophenol triglycidyl compound of the present invention is: [0003] [0004] For its precursor aminophenol, the amino group can be in the para, meta, or ortho position of the phenolic hydroxyl group. [0005] Due to the low viscosity of the aminophenol triglycidyl compound, excellent storage stability, the glass transition temperature of cured molded parts as high as 230 ℃, and the excellent construction performance and heat resistance, this product is widely used as electrical insulating materials, laminates, Adhesives and structural materials, etc. For example: JP.03-21631, 1991-01-30 discloses the use of aminophenol triglycidyl compounds to make carbon fiber composite materials. US Pat.No6,468,659.oct.22, 2002 discloses O,N,N...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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