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Bio-based flexible epoxy resin and preparation method thereof

A flexible epoxy resin and bio-based technology, applied in the field of material chemistry, can solve the problems of heavy odor and high product price, and achieve the effect of reducing glass transition temperature and improving brittleness

Inactive Publication Date: 2019-01-11
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the reason of nitrile rubber, this method has a heavy smell and the price of the product is relatively high

Method used

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  • Bio-based flexible epoxy resin and preparation method thereof
  • Bio-based flexible epoxy resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Levulinic acid and isooctyl alcohol are added in the reactor according to the molar ratio of 1:1, and then catalyst Qs-6 and thioglycolic acid of one-thousandth of the mass of levulinic acid are added, and the molar ratio of Qs-6 to thioglycolic acid is 3:1, react at the reaction temperature of 180°C for 5h, then lower the speed of 7°C / s to 20°C for 20min to obtain isooctyl levulinate. Then isooctyl levulinate and phenol are added in the reaction system according to the molar ratio of 1:4, and catalyst hydrochloric acid and cocatalyst thioglycolic acid are added, and its consumption is according to the molar ratio of hydrochloric acid and isooctyl levulinate of 4:1, thioglycolic acid The molar ratio to isooctyl levulinate is 0.02:1. At 60°C, react for 35 hours, wash with water to remove excess phenol, and obtain bisphenolate ester after drying. Add the obtained bisphenolate ester and epichlorohydrin into the reaction system according to the molar ratio of 1:6, graduall...

Embodiment 2

[0028] Add levulinic acid and isooctyl alcohol into the reactor according to the molar ratio of 1:1, and then add the catalyst p-toluenesulfonic acid and thioglycolic acid which is one percent of the mass of levulinic acid, and the moles of p-toluenesulfonic acid and thioglycolic acid The ratio is 3:1, the reaction temperature is 160°C, react for 3h, then lower the speed of 9°C / s to 22°C and react for 25min to obtain isooctyl levulinate. Then isooctyl levulinate and phenol are added in the reaction system according to the molar ratio of 1:4, and catalyst hydrochloric acid and cocatalyst thioglycolic acid are added, and its consumption is according to the molar ratio of hydrochloric acid and isooctyl levulinate of 4:1, thioglycolic acid The molar ratio to isooctyl levulinate is 0.02:1. At 70°C, react for 25 hours, wash with water to remove excess phenol, and obtain bisphenolate ester after drying. Add the obtained bisphenolate ester and epichlorohydrin into the reaction system...

Embodiment 3

[0034] Add levulinic acid and isooctyl alcohol into the reactor according to the molar ratio of 1:1, and then add catalyst tetrabutyl titanate and thioglycolic acid, which are 1% of the mass of levulinic acid, and tetrabutyl titanate and thioglycolic acid The molar ratio is 4:1, and the reaction temperature is 170° C., reacted for 3 hours, then lowered to 20° C. and reacted for 30 minutes at a rate of 10° C. / s to obtain isooctyl levulinate. Then isooctyl levulinate and phenol are added in the reaction system according to the molar ratio of 1:4, and catalyst hydrochloric acid and cocatalyst thioglycolic acid are added, and its consumption is according to the molar ratio of hydrochloric acid and isooctyl levulinate of 4:1, thioglycolic acid The molar ratio to isooctyl levulinate is 0.02:1. At 70°C, react for 15 hours, wash with water to remove excess phenol, and obtain bisphenolate ester after drying. Add the obtained bisphenolate ester and epichlorohydrin into the reaction sys...

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Abstract

The invention discloses a bio-based flexible epoxy resin and a preparation method thereof. The method comprises the following steps: 1, mixing acetylpropionic acid and long-chain alcohol according toan equal molar ratio, and reacting under the effect of a catalyst so as to obtain iso-octyl levulinate; 2, reacting the iso-octyl levulinate and phenol under the co-action of a catalyst and a promoterso as to obtain esters of diphenolic acid; 3, mixing the esters of diphenolic acid and epoxy chloropropane, dropping an aqueous solution of sodium hydroxide into the mixture, performing reduced pressure distillation after the reaction is ended so as to remove excessive epoxy chloropropane, and performing pickling, alkali washing and drying, thereby obtaining the epoxy resin. The epoxy resin is prepared by replacing acetone with acetylpropionic acid, carboxyl with high activity is introduced, long chains are introduced by virtue of an esterification reaction between the long-chain alcohol andacetylpropionic acid, the glass-transition temperature of the cured epoxy resin is effectively reduced, and the brittleness of the epoxy resin is improved; and the high-purity acetylpropionic acid isprepared by a superposition method by taking glucose, sucrose or cellulose as raw materials.

Description

technical field [0001] The invention belongs to the technical field of material chemistry, and relates to a method for improving the brittleness of epoxy resin. Specifically, the carbon chain is inserted into a long chain through an esterification reaction, and then reacted with phenol to obtain a bisphenolate ester, and finally the bisphenolate ester and epoxy Chloropropane reaction to prepare flexible epoxy resin, that is, bio-based flexible epoxy resin and its preparation method. Background technique [0002] Epoxy resin is widely used in many fields of the market due to its high mechanical strength, good bonding performance and electrical insulation performance. In daily use, it is found that traditional epoxy resins, including epoxy resin 128 and epoxy resin 6101, have defects such as high brittleness, poor low temperature resistance, and impact strength, which severely limit their application in special occasions. [0003] The methods of epoxy resin flexibility curren...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/06
CPCC08G59/063
Inventor 聂小安王义刚董建黄金瑞
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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