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Preparation method for polylactic acid-based epoxy resin

A technology of polylactic acid-based epoxy resin and polylactic acid, which is applied in the field of materials, can solve the problems of slow production rate and high cost, and achieve the effect of simple process, low cost and high production rate

Inactive Publication Date: 2017-12-15
芜湖通全科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, there is no direct utilization of polylactic acid to synthesize epoxy resin in the prior art, and its preparation method has high cost, slow yield and broad prospects

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0022] A preparation method of polylactic acid-based epoxy resin, comprising the following steps:

[0023] Add maleic anhydride to low-molecular-weight polylactic acid, control the reaction temperature at 100-140°C, and react for 2-6 hours under an inert gas atmosphere to obtain polylactic acid terminated by carboxyl groups at both ends;

[0024] The carboxyl-terminated polylactic acid obtained in step (1) is reacted with a halogenated epoxy compound under the action of a basic catalyst to form a polylactic acid halohydrin ester, and the reaction is carried out in the presence of water and an organic solvent, and the reaction temperature is 45~110°C , the reaction time is 0.5~3.0h, the molar ratio of carboxy-terminated polylactic acid to alkali metal catalyst and halogenated epoxy compound is 1:(0.2~0.5):(2.02~20);

[0025] The reaction mixture obtained in step (2) is separated from the water phase, and then an alkali metal catalyst is added until the molar ratio of the ...

Embodiment 1

[0040] Add 300g PDLA (the number average molecular weight is 800) and 50g maleic anhydride to a three-necked 1L flask equipped with stirring and a thermometer, and control the reaction temperature to 100°C. 2 Reaction under atmosphere for 2h.

[0041] Add 200g of chloroform, 200g of water and 150g of epichlorohydrin to a four-necked 1L flask equipped with stirring, thermometer and reflux, heat to 45°C, and mix the product obtained in step (1) with 45g of sodium hydroxide solution ( Concentration 40%) was added into the flask, the feeding time was controlled to be 30 minutes, and the reaction was carried out at 45°C for 2.0h;

[0042] Cool the reaction mixture obtained in step (2) to 40°C, separate the water phase, add 56g of sodium hydroxide and 140g of water, and react at 40°C for 80min;

[0043] Distill the reaction mixture obtained in step (3) at a pressure of 5KPa and a temperature of 120°C, then add 50mL of water for stripping, keep the pressure at 5KPa, and the t...

Embodiment 2

[0046] Add 300g PDLA (the number average molecular weight is 1200) and 48g maleic anhydride to a three-necked 1L flask with stirring and a thermometer, and control the reaction temperature to 130°C. 2 Reaction under atmosphere for 3h.

[0047] Add 200g of chloroform, 200g of water and 150g of epichlorohydrin into a four-necked 1L flask equipped with stirring, thermometer and reflux, heat to 65°C, and mix the product obtained in step (1) with 50g of sodium hydroxide solution ( Concentration 40%) was added into the flask, the feeding time was controlled at 30 minutes, and the reaction was carried out at 80°C for 1.5h;

[0048] Cool the reaction mixture obtained in step (2) to 50°C, separate the water phase, add 60g of sodium hydroxide and 200g of water, and then react at 50°C for 80min;

[0049] Distill the reaction mixture obtained in step (3) at a pressure of 95.4KPa and a temperature of 120°C, and then continue to distill under reduced pressure until the pressure is ...

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Abstract

The invention relates to a preparation method for a polylactic acid-based epoxy resin. Maleic anhydride is used for carrying out end group modification on low-molecular weight polylactic acid, so that polylactic acid, both ends of which are terminated by carboxyl groups, is obtained; the carboxyl-terminated polylactic acid and halogenated epoxy compound react under the action of basic catalyst to generate polylactic acid halogenated alcohol ester; hydrogen halide is then removed, and thereby the polylactic acid-based epoxy resin is obtained. The preparation method has the advantages of simple process, low cost and high yield, and is suitable for mass industrial production; moreover, polylactic acid comes from crops such as corn and potato, which can help to reduce the consumption of petroleum resource and the emission of CO2; and the obtained epoxy resin has lower viscosity and good adhesion, can be used as a matrix for adhesive, coating and composite materials, and is suitable for processes for forming a variety of composite materials.

Description

technical field [0001] The invention relates to the field of materials, in particular to a preparation method of polylactic acid-based epoxy resin. Background technique [0002] Epoxy resin is a polymer oligomer containing two or more epoxy groups, with aliphatic or aromatic backbone, and can react with other active groups to form thermosetting products. Epoxy resin has a large number of active and polar groups. As a thermosetting resin, epoxy resin has excellent comprehensive properties, good adhesion, excellent mechanical properties, small curing shrinkage, good manufacturability, excellent Excellent electrical insulation performance and corrosion resistance performance are widely used in coatings, composite coatings, adhesives, electronic packaging materials, engineering plastics, civil engineering and construction materials and other fields. [0003] The application of epoxy resin is very extensive. The annual consumption of epoxy resin exceeds 1 million tons, and the r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/91C09D163/00C09J163/00C08L63/00
CPCC08G63/912C08L63/00C09D163/00C09J163/00
Inventor 季一全汤佳
Owner 芜湖通全科技有限公司
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