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Halogen-free flame-retardant bio-based epoxy resin precursor and preparation method and application thereof

A technology based on epoxy resin and epoxy resin, applied in the direction of epoxy resin glue, epoxy resin coating, adhesive type, etc., can solve the problems of unsuitability for industrial production, harsh reaction conditions, complicated preparation methods, etc. The effect of reducing dependence on petrochemical resources and its pollution to the environment, controllable reaction conditions, and simplification of reaction steps

Active Publication Date: 2019-04-19
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

[0006] The preparation method of the above invention is complicated, the reaction conditions are harsh, and the raw materials that can be used are single, which is not suitable for industrial production. In view of the above problems, the present invention provides a simple preparation method, wide source of raw materials, excellent performance, and a bisphenol structure that can replace Novel halogen-free flame retardant bio-based epoxy resin precursor of petroleum-based bisphenol-based epoxy

Method used

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  • Halogen-free flame-retardant bio-based epoxy resin precursor and preparation method and application thereof
  • Halogen-free flame-retardant bio-based epoxy resin precursor and preparation method and application thereof
  • Halogen-free flame-retardant bio-based epoxy resin precursor and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0035] (1) Dissolve 0.1mol vanillin, 0.1mol DOPO and 0.003mol p-toluenesulfonic acid in 0.5mol guaiacol at 130°C, and react at 130°C for 24 hours to obtain bisphenol biobased phosphorus-containing mono body with a yield of 84%.

[0036] (2) React 0.1 mol bisphenol bio-based phosphorus-containing monomer and 1 mol epichlorohydrin in the presence of 0.003 mol tetrabutylammonium bromide at 80°C for 6 hours, then remove the solvent by rotary evaporation under reduced pressure, wash with acetone and dry Finally, epoxidized bio-based bisphenols were obtained with a yield of 89%.

[0037] The specific reaction formula is:

[0038]

[0039] H NMR spectrum 1 H-NMR such as figure 1As shown, there is a one-to-one correspondence between each peak on the figure and the atoms on the structure of the epoxidized bio-based bisphenol compound.

[0040] The obtained epoxidized bio-based bisphenol compound and the curing agent DDM are uniformly mixed in a molten state according to the mola...

Embodiment 2

[0043] (1) Dissolve 0.1mol o-vanillin, 0.1mol DOPO and 0.003mol p-toluenesulfonic acid in 0.5mol guaiacol at 130°C, and react at 130°C for 24h to obtain bio-based bisphenol mono body with a yield of 87%.

[0044] (2) React 0.1 mol of the above monomer and 1 mol of epichlorohydrin in the presence of 0.02 mol of tetrabutylammonium bromide at 80°C for 6 hours, then remove the solvent by rotary evaporation under reduced pressure, wash with acetone and dry to obtain epoxidized Bio-based bisphenols with a yield of 86%.

[0045] The obtained epoxidized bio-based bisphenol compound and the curing agent DDM are uniformly mixed in a molten state according to the molar ratio of epoxy and NH one to one, then heated and pre-cured in a blast oven, and finally heated in a vacuum oven at 250 ℃ for post-curing for 5 hours to obtain a bio-based bisphenol epoxy-DDS epoxy resin cured product.

[0046] The obtained cured product has a glass transition temperature of 225° C., a Td10% of 385° C., ...

Embodiment 3

[0048] (1) Dissolve 0.1mol salicylaldehyde, 0.1mol DOPO and 0.002mol p-toluenesulfonic acid in 0.4mol guaiacol at 140°C, and react at 140°C for 18h to obtain bisphenol biobased phosphorus-containing Monomer, yield 82%.

[0049] (2) React 0.1 mol of bisphenol bio-based phosphorus-containing monomer and 1 mol of epichlorohydrin in the presence of 0.02 mol of tetrabutylammonium bromide at 80°C for 6 hours, then remove the solvent by rotary evaporation under reduced pressure, wash with acetone and dry Finally, epoxidized bio-based bisphenols were obtained with a yield of 88%.

[0050] The obtained epoxidized bio-based bisphenol compound and the curing agent DDM are uniformly mixed in a molten state according to the molar ratio of epoxy and NH one to one, then heated and pre-cured in a blast oven, and finally heated in a vacuum oven at 250 ℃ for post-curing for 5 hours to obtain a bio-based bisphenol epoxy-DDS epoxy resin cured product.

[0051] The obtained cured product has a g...

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Abstract

The invention discloses a halogen-free flame-retardant bio-based epoxy resin precursor and its preparation method. The preparation method comprises the following steps: firstly, a bio-based phenol monomer, a phosphorus-containing monomer and an aldehyde-containing bio-based phenol monomer are subjected to a simple condensation reaction; and then, the product is subjected to an epoxidation reactionto prepare the halogen-free flame-retardant bio-based epoxy resin precursor. The preparation method has simple process, is simple to operate, has good controllability, is easy to implement, and is suitable for large-scale industrial production. By preparing thermosetting epoxy resin from the bio-based epoxy resin precursor and an amine or anhydride curing agent, the modified epoxy resin can haveexcellent thermal property, mechanical property and flame retardant property, has the possibility of replacing the existing petroleum base products, and has a wider range of application.

Description

technical field [0001] The invention belongs to the field of bio-based thermosetting epoxy resins, and in particular relates to a halogen-free flame-retardant bio-based epoxy resin precursor and a preparation method and application thereof. Background technique [0002] Epoxy resin refers to the general term for a class of polymers containing two or more epoxy groups in the molecular structure. It is the polycondensation product of epichlorohydrin and bisphenol A or other polyols. Due to the high chemical activity of the epoxy group in its structure, it can react with a variety of compounds containing active hydrogen, thereby curing and crosslinking to form a network structure, so it is a thermosetting resin. Epoxy resin is a general-purpose thermosetting resin with a very wide range of uses. It is widely used in aerospace, coatings, adhesives, circuit packaging and other fields because of its excellent comprehensive properties. It is a very important class of polymer mater...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/06C08G59/30C08G59/50C09J163/00C09D163/00
CPCC08G59/06C08G59/304C08G59/5033C09D163/00C09J163/00
Inventor 刘敬楷代金月刘小青朱锦王静刚王帅朋
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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