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A kind of bio-based flame retardant epoxy resin precursor based on natural phenolic monomer and its preparation method and application

An epoxy resin, bio-based technology, applied in the direction of organic chemistry, can solve the problems that epoxy resin is not a pure bio-based, green, environmentally friendly product, complex preparation method, harsh reaction conditions, etc., to achieve sustainable sources The development and synthesis steps are simple, and the mechanical properties and flame retardant properties are good

Active Publication Date: 2020-08-11
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, in order to make the epoxy resin have a flame-retardant effect, the above-mentioned preparation method needs to use the active group on the gallic acid to introduce phosphorus-containing monomers. The preparation method is complicated and the reaction conditions are harsh. The obtained epoxy resin does not actually belong to a pure biological basic, green and environmental protection products

Method used

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  • A kind of bio-based flame retardant epoxy resin precursor based on natural phenolic monomer and its preparation method and application
  • A kind of bio-based flame retardant epoxy resin precursor based on natural phenolic monomer and its preparation method and application
  • A kind of bio-based flame retardant epoxy resin precursor based on natural phenolic monomer and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Dissolve 1mol of salicylaldehyde, 0.5mol of paraformaldehyde, and 0.01mol of sulfuric acid in 200mL of anhydrous acetic acid, react at 60°C for 40 hours, remove the solvent by rotary evaporation under reduced pressure, wash with water and dry to obtain dihydrate Popylaldehyde compound, the productive rate is 89%;

[0034] (2) React 1mol disalicylaldehyde compound and 10mol epichlorohydrin in the presence of 0.1mol tetrabutylammonium bromide at 80°C for 12 hours, then remove the solvent by rotary evaporation under reduced pressure, wash with water and dry The epoxidized disalicylaldehyde compound was obtained with a yield of 95%.

[0035] The proton nuclear magnetic resonance spectrum of the disalicylaldehyde compound that step (1) obtains 1 H-NMR such as figure 1 As shown, each peak on the figure is in one-to-one correspondence with the hydrogen atoms on the structure of the disalicylaldehyde compound.

[0036] The proton nuclear magnetic resonance spectrum of th...

Embodiment 2

[0040] (1) Dissolve 1mol of salicylaldehyde, 0.2mol of paraformaldehyde, and 0.01mol of sulfuric acid in 220mL of anhydrous acetic acid, react at 70°C for 35 hours, remove the solvent by rotary evaporation under reduced pressure, wash with water and dry to obtain dihydrate Poplaric aldehyde compound, the productive rate is 81%;

[0041](2) React 1 mol of disalicylaldehyde compound and 5 mol of epichlorohydrin in the presence of 0.5 mol of tetrabutylammonium bromide at 100°C for 6 hours, then remove the solvent by rotary evaporation under reduced pressure, wash with water and dry The epoxidized disalicylaldehyde compound was obtained with a yield of 97%.

[0042] The epoxidized disalicylaldehyde compound obtained and the curing agent m-phenylenediamine are mixed uniformly according to the molar ratio of epoxy and amino group one to two and aldehyde group and amino group one to one respectively in the blast oven, as follows Temperature program curing: curing at 80°C for 2 hours...

Embodiment 3

[0045] (1) Dissolve 1mol of salicylaldehyde, 0.4mol of paraformaldehyde, and 0.03mol of sulfuric acid in 260mL of anhydrous acetic acid, react at 80°C for 24 hours, remove the solvent by rotary evaporation under reduced pressure, wash with water and dry to obtain dihydrate Poplaric aldehyde compound, the productive rate is 91%;

[0046] (2) React 1 mol of disalicylaldehyde compound and 8 mol of epichlorohydrin in the presence of 0.3 mol of tetrabutylammonium bromide at 90°C for 8 hours, then remove the solvent by rotary evaporation under reduced pressure, wash with water and dry The epoxidized disalicylaldehyde compound was obtained with a yield of 95%.

[0047] Mix the obtained epoxidized disalicylaldehyde compound and curing agent ethylenediamine according to the molar ratio of epoxy and amino group one to two and aldehyde group and amino group one to one respectively, and then heat up in a blast oven as follows Programmed temperature curing: curing at 80°C for 2 hours, 120...

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Abstract

The invention discloses a biology-based flame-retardant epoxy resin precursor on the basis of natural phenol monomers. The biology-based flame-retardant epoxy resin precursor is of a structure shown as a following formula (I). A method for preparing the biology-based flame-retardant epoxy resin precursor includes carrying out two-step reaction on the natural phenol monomers, trioxymethylene and epichlorohydrin to obtain the biology-based high-performance flame-retardant epoxy resin precursor on the basis of the natural phenol monomers. The biology-based flame-retardant epoxy resin precursor and the method have the advantages that processes for preparing the biology-based flame-retardant epoxy resin precursor are simple, methods for operating the biology-based flame-retardant epoxy resin precursor are simple and convenient, and the biology-based flame-retardant epoxy resin precursor and the method are good in controllability, easy to implement and applicable to large-scale industrial production; thermoset epoxy resin prepared from the biology-based high-performance flame-retardant epoxy resin precursor on the basis of the natural phenol monomers and amine curing agents is excellentin flame retardance and mechanical property and wide in use range, and existing petroleum-based products can be possibly replaced with the thermoset epoxy resin.

Description

technical field [0001] The invention relates to the field of bio-based thermosetting epoxy resins, in particular to a bio-based flame retardant epoxy resin precursor and its preparation method and application. Background technique [0002] Epoxy resin is a thermosetting resin with a wide range of uses. It is widely used in anti-corrosion coatings, adhesives, microelectronics, aerospace and other fields because of its excellent comprehensive properties. It is a very important class of thermosetting materials. However, at this stage, most epoxy resins are derived from petroleum resources, and petroleum resources are an unsustainable resource. With the decreasing reserves, the cost of polymer materials derived from petroleum resources will inevitably increase. high. [0003] Recently, under the dual pressure of protecting the environment and saving petroleum resources, bio-based polymer materials using sustainable resources as raw materials have entered people's field of visio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D301/02C07D303/27C08G59/24
Inventor 代金月腾娜刘小青王静刚朱锦
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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