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A preparation method of single-component photoinitiated self-healing silica-based microcapsules

A silicon dioxide and light-initiated technology, which is applied in the direction of silicon dioxide, microcapsule preparations, silicon oxide, etc., can solve the problems of atomic oxygen damage and failure, and achieve improved strength, good weather resistance and temperature resistance, and flexible formulations Effect

Active Publication Date: 2018-12-28
湖北金伟新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the currently developed single-component microcapsules are prone to failure due to atomic oxygen damage in space environments because their initiators are free radical initiators.

Method used

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  • A preparation method of single-component photoinitiated self-healing silica-based microcapsules
  • A preparation method of single-component photoinitiated self-healing silica-based microcapsules

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Mix 1g of bisphenol A type epoxy resin E-51, 1g of alicyclic epoxy resin A1815, 0.4g of cationic photoinitiator PI6992 and 1g of tetraethyl orthosilicate as the oil phase, and mix it with 40mL of 2% non- The aqueous solution of ionic surfactant F-127 was mixed and stirred by 8000rpm high-speed homogenizer for 15min to form an O / W emulsion; transfer the O / W emulsion to a round bottom flask and add 400μL pre-prepared 2mol / L Dilute hydrochloric acid solution, heat up to 50°C, start the reaction at 300rpm, after 3 hours, add 1mL tetraethyl orthosilicate, and add 400μL 2mol / L dilute hydrochloric acid solution every 4 hours, add a total of 3 times, continue the reaction for 12h, After the reaction is complete, wash with deionized water several times until the supernatant is colorless and transparent, and place it in an oven to dry.

Embodiment 2

[0017] Mix 1g of bisphenol A type epoxy resin E-51, 1g of alicyclic epoxy resin A1815, 0.6g of cationic photoinitiator PI6992 and 1g of tetraethyl orthosilicate as the oil phase, and mix with 40mL of 2% non- The aqueous solution of ionic surfactant F-127 was mixed and stirred by 8000rpm high-speed homogenizer for 15min to form an O / W emulsion; transfer the O / W emulsion to a round bottom flask and add 500μL pre-prepared 2mol / L Dilute hydrochloric acid solution, heat up to 50°C, start reaction at 300rpm, after 3 hours, add 1.5mL tetraethyl orthosilicate, and add 500μL dilute hydrochloric acid solution with a concentration of 2mol / L every 4 hours, add 3 times in total, Continue to react for 12 hours. After the reaction is complete, wash with deionized water several times until the supernatant is colorless and transparent, and place it in an oven to dry.

[0018] like figure 1 As shown, it can be seen that the surface of the prepared microcapsules is relatively dense, the particl...

Embodiment 3

[0021] Mix 1g of bisphenol A type epoxy resin E-51, 1g of alicyclic epoxy resin A1815, 0.8g of cationic photoinitiator PI6992 and 1g of tetraethyl orthosilicate as the oil phase, and mix them with 40mL of 2% non- The aqueous solution of ionic surfactant F-127 was mixed and stirred by a high-speed homogenizer at 8000 rpm for 15 minutes to form an O / W emulsion. Transfer the O / W emulsion to a round bottom flask, add 600 μL of pre-prepared 2mol / L dilute hydrochloric acid solution dropwise, raise the temperature to 50°C, and start the reaction at a speed of 300rpm. After 3 hours, add 1.5mL tetraethyl orthosilicate At the same time, add 600 μL of dilute hydrochloric acid solution with a concentration of 2mol / L every 4 hours, add a total of 3 times, continue to react for 12 hours, after the reaction is complete, wash with deionized water for several times until the supernatant is colorless and transparent, and place it in an oven to dry .

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Abstract

The invention discloses a preparation method of a single-component photo-initiation self-healing silicon dioxide-based microcapsule. The preparation method comprises following steps: epoxy resin, a cationic photoinitiator, and tetraethyl orthosilicate are uniformly mixed at a mass ratio of 2:0.4-1:1-2 as an oil phase; the oil phase mixture is mixed with an aqueous solution of a nonionic surfactant, and an obtained mixed material is subjected to stirring for 15min using a high-speed homogenizer at a speed of 8000rpm so as to obtain an O / W emulsion; the O / W emulsion is delivered into a container, diluted hydrochloric acid is added dropwise, the container is delivered into an oil bath pan, the temperature is increased to 50 DEG C, and reaction is carried out at a revolving speed of 300rpm; 3h later, tetraethoxysilane is added, a hydrochloric acid solution is added every 4h for three times, continuous reaction is carried out for 12h, an obtained product is washed with deionized water for a plurality of times until an obtained supernatant liquid is colorless and transparent, and then the product is delivered into a drying oven for drying. The single-component photo-initiation self-healing silicon dioxide-based microcapsule possesses monodispersity, high coating rate, and excellent thermal stability; and stability and repair rate are increased at a certain degree.

Description

technical field [0001] The invention relates to a preparation method of microcapsules, in particular to a preparation method of silicon dioxide-based microcapsules. Background technique [0002] Functional polymer composites have attracted extensive attention in the field of spacecraft coatings due to their light weight, good flexibility, and easy processing. However, when the spacecraft operates in the harsh space environment for a long time, the coating is subject to the combined effects of high and low temperature thermal cycles, low air pressure, atomic oxygen, charged particles, and ultraviolet radiation, which easily cause microcracks, which then expand and even lead to failure. . Self-healing materials provide a feasible idea for extending the service life of the coating, which can enable the coating to repair itself when damaged, thereby improving the operational reliability of the spacecraft and extending its service life. Among them, the microcapsule self-healing...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/02C01B33/12
CPCB01J13/02C01B33/12
Inventor 郭万春贾茵田克松徐朝鹏焦姣李瑞飞吴月豪曹玲王海燕
Owner 湖北金伟新材料有限公司
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