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Bio-based epoxy resin emulsifier as well as water-based emulsion and preparation method thereof

A technology based on epoxy resin and gallic acid-based epoxy resin, which is applied in the field of bio-based epoxy resin emulsifier and its water-based emulsion and preparation, can solve problems such as difficulty in meeting green environmental protection requirements, ecological environmental hazards, etc. Effects that are conducive to sustainable development

Active Publication Date: 2020-09-01
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the traditional solvent-based epoxy resin, because it contains a large amount of organic solvents, brings harm to the ecological environment, and it is increasingly difficult to meet the market's requirements for green environmental protection

Method used

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  • Bio-based epoxy resin emulsifier as well as water-based emulsion and preparation method thereof
  • Bio-based epoxy resin emulsifier as well as water-based emulsion and preparation method thereof
  • Bio-based epoxy resin emulsifier as well as water-based emulsion and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Preparation of emulsifier GAE-nDOPO-(4-n)(MEA-PEGGE-MEA-PEGGE)(n=2):

[0033](1) Preparation of GAE and GAE-2DOPO adduct solution: first add gallic acid (27.2g, 0.16mol) and epichlorohydrin (355.2g, 3.84 mol), stirring and heating for 30 minutes, adding 3.84g of tetrabutylammonium bromide (TBAB) as a catalyst, gradually warming up to 105°C, after reacting for 6 hours, recovering excess epichlorohydrin by distillation under reduced pressure, and then adding 160 gram of ethyl acetate solvent, adjust the temperature to 25°C and add NaOH (25.6g, 0.64mol) solution (40% mass aqueous solution) for ring closure reaction for 2 hours, then transfer the reaction solution to a separatory funnel and wash it with water for 3 times To neutrality, let it stand, separate the water layer, and distill the oil layer product under reduced pressure to obtain a light yellow semi-solid epoxy resin (GAE, its epoxy value is 0.68). Get homemade gallic acid-based epoxy resin (GAE) 11.76g, DOPO 8....

Embodiment 2

[0050] Preparation of emulsifier GAE-nDOPO-(4-n)(MEA-PEGGE-MEA-PEGGE)(n=3):

[0051] (1) Preparation of GAE and GAE-3DOPO adduct solution: first add gallic acid (27.2g, 0.16mol) and epichlorohydrin (355.2g, 3.84 mol), stirring and heating for 30 minutes, adding 3.84g of tetrabutylammonium bromide (TBAB) as a catalyst, gradually warming up to 105°C, after reacting for 6 hours, recovering excess epichlorohydrin by vacuum distillation, and then adding 160g ethyl acetate solvent, adjust the temperature to 25°C and add NaOH (25.6g, 0.64mol) solution (40% mass aqueous solution) for ring closure reaction for 2 hours, then transfer the reaction solution to a separatory funnel and wash with water for 3-4 Secondary to neutral, stand still, separate the water layer, and the oil layer product is distilled under reduced pressure to obtain a light yellow semi-solid epoxy resin (GAE, its epoxy value is 0.68). Get homemade gallic acid base epoxy resin (GAE) 23.52g, DOPO 25.92g as mentioned a...

Embodiment 3

[0063] Preparation of emulsifier GAE-nDOPO-(4-n)(MEA-PEGGE-MEA-PEGGE)(n=1):

[0064] (1) Preparation of GAE and GAE-1DOPO adduct solution: first add gallic acid (27.2g, 0.16mol) and epichlorohydrin (355.2g, 3.84 mol), stirring and heating for 30 minutes, adding 3.84g of tetrabutylammonium bromide (TBAB) as a catalyst, gradually warming up to 105°C, after reacting for 6 hours, recovering excess epichlorohydrin by vacuum distillation, and then adding 160g ethyl acetate solvent, adjust the temperature to 25°C and add NaOH (25.6g, 0.64mol) solution (40% mass aqueous solution) for ring closure reaction for 2 hours, then transfer the reaction solution to a separatory funnel and wash with water for 3 times to Neutral, let stand, separate the water layer, and distill the oil layer product under reduced pressure to obtain light yellow semi-solid epoxy resin (GAE, its epoxy value is 0.68). Get homemade gallic acid-based epoxy resin (GAE) 11.76g, DOPO 4.32g as mentioned above, catalyst ...

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Abstract

The invention discloses a bio-based epoxy resin emulsifier. The emulsifier structurally comprises a hydrophobic gallic acid-based epoxy resin molecular chain segment, a hydrophilic flexible polyetheralcohol amine multi-block chain segment and a phosphorus-containing DOPO molecular chain segment. Therefore, the gallic acid-based epoxy resin can be well emulsified under an aqueous condition. The invention also discloses a water-based emulsion obtained by emulsifying gallic acid-based epoxy resin with the emulsifier and a preparation method of the water-based emulsion. The prepared water-based emulsion is stable and small in particle size and has a flame-retardant function.

Description

technical field [0001] The invention relates to the technical field of epoxy resins, in particular to a bio-based epoxy resin emulsifier, an aqueous emulsion and a preparation method thereof. Background technique [0002] Epoxy resin materials have the advantages of excellent adhesive properties, electrical insulation properties, low shrinkage, high strength and high modulus, making them play an important role in the fields of electronics, ships, aerospace, and machinery manufacturing. Traditional petroleum-based derivative type epoxy resins such as bisphenol A epoxy resins, the raw material bisphenol A required for its preparation is a petroleum derivative, which needs to consume a large amount of non-renewable petroleum resources; and bisphenol A is considered to be harmful to A chemical that poses a potential hazard to human health. Due to the increasing shortage of petroleum resources and the increasing awareness of sustainable development, it has become an irreversible...

Claims

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Application Information

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IPC IPC(8): C08J3/03C08L63/00
CPCC08J3/03C08J2363/00C08J2463/00
Inventor 周继亮张俊珩张道洪李廷成
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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