Preparation method of bio-based epoxy resins based on natural Magnolia officinalis derivative

A technology based on epoxy resin and epoxy resin, which is applied in the field of preparation of bio-based high-performance epoxy resin, can solve the problems of reducing the thermal stability and mechanical properties of the system, difficulty in achieving high aromatization, and poor comprehensive performance. Achieve the effect of being suitable for large-scale production, the synthesis method is simple and efficient, and easy to implement

Active Publication Date: 2019-11-05
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are usually some weak bonds or flexible aliphatic chains and alicyclic structures in the structure of the currently prepared bio-based epoxy resin, which reduces the thermal stability and mechanical properties of the system.
Moreover, most bio-based epoxy resin structures are difficult to achieve a high degree of aromatization, so its comprehensive performance is still inferior to that of bisphenol A epoxy resin.
[0005] In addition, both petroleum-based epoxy resins and bio-based epoxy resins currently have the disadvantage of poor flame retardancy, which has become another key issue that limits the application of epoxy resins.

Method used

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  • Preparation method of bio-based epoxy resins based on natural Magnolia officinalis derivative
  • Preparation method of bio-based epoxy resins based on natural Magnolia officinalis derivative
  • Preparation method of bio-based epoxy resins based on natural Magnolia officinalis derivative

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Experimental program
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Effect test

Embodiment 1

[0030](1) The synthesis of magnolol difunctionality epoxy resin: 10g magnolol, 35g epichlorohydrin, 0.42g benzyltriethylammonium chloride are added in the there-necked flask successively, under nitrogen atmosphere, be heated up to React at 100° C. for 5 hours, then take 4.5 g of sodium hydroxide to prepare an aqueous solution of sodium hydroxide with a concentration of 30 wt%, and add it dropwise into the reaction system, and continue to react for 3 hours. After the reaction, the reaction system was washed three times with distilled water, and the organic layer was separated. After drying, excess epichlorohydrin was distilled off under reduced pressure to obtain a magnolol difunctional epoxy resin.

Embodiment 2

[0032] (2) Synthesis of honokiol difunctional epoxy resin: 10g honokiol, 52g epichlorohydrin, and 2.1g benzyltriethylammonium chloride were added to a three-necked flask successively, under a nitrogen atmosphere , the temperature was raised to 120° C. for 5 hours, and then 4.5 g of sodium hydroxide was taken to form a 50 wt % sodium hydroxide aqueous solution, which was added dropwise to the reaction system, and the reaction was continued for 2.5 hours. After the reaction, the system was washed with distilled water for 3 times, and several layers were separated and dried, then distilled under reduced pressure to remove excess epichlorohydrin to obtain honokiol difunctional epoxy resin.

Embodiment 3

[0034] (3) Synthesis of magnolol tetrafunctional epoxy resin: 15g magnolol difunctional epoxy resin is dissolved in 35g methylene chloride, the system is placed in an ice-water bath, and 6.8g m-chlorine is slowly added thereto Peroxybenzoic acid, then, the system was heated to 50 ° C for 48 hours, after the reaction, the reaction system was washed with sodium sulfite aqueous solution and sodium carbonate aqueous solution for 3 times, the organic layer was separated, dried, and the solvent was removed by distillation under reduced pressure. Obtain magnolol tetrafunctional epoxy resin.

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Abstract

The invention belongs to the technical field of bio-based thermosetting epoxy resins, and discloses a preparation method of bio-based epoxy resins based on a natural Magnolia officinalis derivative. The preparation method comprises the following steps: the natural Magnolia officinalis derivative and epichlorohydrin undergo a one-step reaction to obtain a corresponding natural Magnolia officinalisderivative difunctional epoxy resin; and the difunctional epoxy resin is oxidized by m-chloroperoxybenzoic acid to obtain the corresponding natural Magnolia officinalis derivative tetrafunctional epoxy resin. The entire synthesis process is very simple and efficient, so large-scale production is easy. The bio-based difunctional and tetrafunctional epoxy resins based on the natural Magnolia officinalis derivative have the advantages of excellent heat resistance, excellent mechanical properties and excellent flame retardancy, and have great potential when used to replace petroleum-based bisphenol A epoxy resin.

Description

technical field [0001] The invention belongs to the technical field of bio-based thermosetting epoxy resins, and in particular relates to a preparation method of bio-based high-performance epoxy resins based on natural Magnolia officinalis derivatives. Background technique [0002] As one of the three major thermosetting resins, epoxy resin has excellent comprehensive properties and is widely used in many fields such as coatings, adhesives, electronic packaging materials, and high-performance composite materials. [0003] However, most of the current commercial epoxy resins are produced from petroleum raw materials, and bisphenol A epoxy resins account for more than 90% of the total output of epoxy resins. Although one of its raw materials, epichlorohydrin, can be produced from biomass raw material glycerin, but another main raw material, bisphenol A, can only be produced from petroleum raw materials at present. Petroleum is a non-renewable resource, which has been consumed...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/24C08G59/32C08G59/50C07D301/28C07D303/27C07D303/30
CPCC08G59/245C08G59/3218C08G59/504C07D303/27C07D303/30C07D301/28
Inventor 蹇锡高翁志焕王锦艳张守海刘程戚裕
Owner DALIAN UNIV OF TECH
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