Preparation process for core-shell nanoparticle emulsion for impact modification of aqueous epoxy resin

Abstract

The present invention discloses a preparation process for a core-shell nanoparticle emulsion for impact modification of aqueous epoxy resin. The preparation method comprises the following steps of: step A, using a sol-gel method to prepare uniformly dispersed nanosilica, and using a silane coupling agent to conduct surface hydrophobic modification on the nanosilica to obtain hydrophobic nanosilica; and step B, using a micro-suspended seed emulsion polymerization method and the hydrophobic nanosilica obtained in step A as a core structure, and using methacrylate and a glycidyl methacrylate monomer to conduct polymer coating to obtain the product. Core-shell structure nanoparticles prepared by the preparation process, using silica as the core with the surface coated with polymers, have the advantages of high coating rate, uniform size and same shell thickness.

Description

technical field

[0001] The invention belongs to the field of water-based epoxy resin toughening agents, and in particular relates to a preparation process of core-shell nanoparticle emulsion for water-based epoxy resin impact modification. Background technique

[0002] Epoxy resin is a three-dimensional network thermosetting polymer and a very brittle material. Its toughening modification is an important topic in basic research and application development in the field of polymer science and materials, and has always received extensive attention. . But pure rubber or elastomer toughening or rigid particles have some disadvantages in toughening epoxy resin. For pure rubber or elastomer toughened polymers, although the impact toughness has been greatly improved, it is usually necessary to add 10wt%-20wt% rubber or elastomer, which often leads to too much loss of strength and modulus of the material; and Using inorganic rigid particles to toughen it, although the strength and ...

Examples

Embodiment 1

[0049] A. Measure 45 parts of ethanol, 25 parts of deionized water and 10 parts of ammonia water into a reactor with a magnetic stirring device and stir for 10 minutes at a speed of 300 rpm, then increase the speed to 1000 rpm, and measure Mix 15 parts of ethanol and 4.5 parts of tetraethyl orthosilicate evenly, and then quickly drop the mixed solution into the reactor. After the color of the mixed solution in the reactor changes from transparent to milky white, reduce the rotating speed to 300 rpm, keep React at this speed for 4 hours; continue to stir and adjust the temperature to 40-50°C, then add 2 parts of silane coupling agent to the system, keep stirring at the temperature for 24 hours, and then put the dispersion in a 50°C blast drying oven to dry to powder state, and then dried in a vacuum oven at 80°C for 24 hours, then centrifuged and washed with ethanol for 3-4 times, and finally dried to obtain modified hydrophobic nano-silica particles.

[0050] product testing: ...

Embodiment 2

[0059] A. Measure 45 parts of ethanol, 25 parts of deionized water and 10 parts of ammonia water into a reactor with a magnetic stirring device and stir at a speed of 300 rpm for 10 minutes, while measuring 15 parts of ethanol and 4.5 parts of ethyl orthosilicate Mix the esters evenly, then drop the mixture into the reactor with a dropping funnel at a rate of 2ml / min, and react for 4 hours after the dropwise addition; continue to stir and adjust the temperature to 40-50°C, and then add 2 parts of The silane coupling agent is kept at a stirring temperature for 24 hours, centrifuged and washed with ethanol for 3-4 times, and finally dried to obtain modified hydrophobic nano-silica particles.

[0060] product testing:

[0061] 1. Electron microscope test, take 0.02g of the nano-silica particles prepared above into 10ml of absolute ethanol, ultrasonically disperse for 30 minutes, and then drop them on the silicon wafer, and observe with the scanning electron microscope after the e...

Embodiment 3

[0067] A. Measure 45 parts of ethanol, 30 parts of deionized water and 10 parts of ammonia water into a reactor with a magnetic stirring device and stir at a speed of 300 rpm for 10 minutes, then increase the speed to 1000 rpm, and measure Mix 15 parts of ethanol and 3 parts of tetraethyl orthosilicate evenly, and then quickly drop the mixed solution into the reactor. After the color of the mixed solution in the reactor changes from transparent to milky white, reduce the rotating speed to 300 rpm, keep React at this speed for 4 hours; continue to stir and adjust the temperature to 40-50°C, then add 2 parts of silane coupling agent to the system, keep stirring at the temperature for 24 hours, and then put the dispersion in a 50°C blast drying oven to dry to powder state, and then dried in a vacuum oven at 80°C for 24 hours, then centrifuged and washed with ethanol for 3-4 times, and finally dried to obtain modified hydrophobic nano-silica particles;

[0068] B. Add 400 parts of...

technical field

[0001] The invention belongs to the field of water-based epoxy resin toughening agents, and in particular relates to a preparation process of core-shell nanoparticle emulsion for water-based epoxy resin impact modification. Background technique

[0002] Epoxy resin is a three-dimensional network thermosetting polymer and a very brittle material. Its toughening modification is an important topic in basic research and application development in the field of polymer science and materials, and has always received extensive attention. . But pure rubber or elastomer toughening or rigid particles have some disadvantages in toughening epoxy resin. For pure rubber or elastomer toughened polymers, although the impact toughness has been greatly improved, it is usually necessary to add 10wt%-20wt% rubber or elastomer, which often leads to too much loss of strength and modulus of the material; and Using inorganic rigid particles to toughen it, although the strength and ...

Examples

Embodiment 1

[0049] A. Measure 45 parts of ethanol, 25 parts of deionized water and 10 parts of ammonia water into a reactor with a magnetic stirring device and stir for 10 minutes at a speed of 300 rpm, then increase the speed to 1000 rpm, and measure Mix 15 parts of ethanol and 4.5 parts of tetraethyl orthosilicate evenly, and then quickly drop the mixed solution into the reactor. After the color of the mixed solution in the reactor changes from transparent to milky white, reduce the rotating speed to 300 rpm, keep React at this speed for 4 hours; continue to stir and adjust the temperature to 40-50°C, then add 2 parts of silane coupling agent to the system, keep stirring at the temperature for 24 hours, and then put the dispersion in a 50°C blast drying oven to dry to powder state, and then dried in a vacuum oven at 80°C for 24 hours, then centrifuged and washed with ethanol for 3-4 times, and finally dried to obtain modified hydrophobic nano-silica particles.

[0050] product testing: ...

Embodiment 2

[0059] A. Measure 45 parts of ethanol, 25 parts of deionized water and 10 parts of ammonia water into a reactor with a magnetic stirring device and stir at a speed of 300 rpm for 10 minutes, while measuring 15 parts of ethanol and 4.5 parts of ethyl orthosilicate Mix the esters evenly, then drop the mixture into the reactor with a dropping funnel at a rate of 2ml / min, and react for 4 hours after the dropwise addition; continue to stir and adjust the temperature to 40-50°C, and then add 2 parts of The silane coupling agent is kept at a stirring temperature for 24 hours, centrifuged and washed with ethanol for 3-4 times, and finally dried to obtain modified hydrophobic nano-silica particles.

[0060] product testing:

[0061] 1. Electron microscope test, take 0.02g of the nano-silica particles prepared above into 10ml of absolute ethanol, ultrasonically disperse for 30 minutes, and then drop them on the silicon wafer, and observe with the scanning electron microscope after the e...

Embodiment 3

[0067] A. Measure 45 parts of ethanol, 30 parts of deionized water and 10 parts of ammonia water into a reactor with a magnetic stirring device and stir at a speed of 300 rpm for 10 minutes, then increase the speed to 1000 rpm, and measure Mix 15 parts of ethanol and 3 parts of tetraethyl orthosilicate evenly, and then quickly drop the mixed solution into the reactor. After the color of the mixed solution in the reactor changes from transparent to milky white, reduce the rotating speed to 300 rpm, keep React at this speed for 4 hours; continue to stir and adjust the temperature to 40-50°C, then add 2 parts of silane coupling agent to the system, keep stirring at the temperature for 24 hours, and then put the dispersion in a 50°C blast drying oven to dry to powder state, and then dried in a vacuum oven at 80°C for 24 hours, then centrifuged and washed with ethanol for 3-4 times, and finally dried to obtain modified hydrophobic nano-silica particles;

[0068] B. Add 400 parts of...

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