Preparation method of photosensitive particle stabilizing emulsion as well as preparation method of thin-wall hollow sphere

A photosensitive, hollow sphere technology, applied in the field of porous ceramic materials, can solve the problems of high production cost, limited preparation parameters, difficult mass production, etc., and achieves the effects of low cost, favorable industrial production and strong stability

Active Publication Date: 2018-10-02
TSINGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the current existing technology, the preparation methods of ceramic hollow microspheres mainly include spray drying method, sacrificial template method, sol-gel method, melting method, etc., but these methods have limited preparation parameters, high production costs, and difficulty in mass production. And other issues

Method used

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  • Preparation method of photosensitive particle stabilizing emulsion as well as preparation method of thin-wall hollow sphere
  • Preparation method of photosensitive particle stabilizing emulsion as well as preparation method of thin-wall hollow sphere
  • Preparation method of photosensitive particle stabilizing emulsion as well as preparation method of thin-wall hollow sphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Preparation of oil-in-water photosensitive particle stabilized emulsion:

[0038] (1) Water phase: Prepare 30 g of water-based alumina ceramic slurry with a solid phase content of 52 wt%, wherein the average particle size of alumina is 0.5 μm, add 0.1 g of valeric acid, and adjust the pH to 4.8;

[0039] (2) Oil phase: after mixing 35g polyurethane acrylate and pentaerythritol tetraacrylate with a mass ratio of 3:2, add 819 photoinitiators of 2wt% resin quality;

[0040] (3) Emulsification: Mix the water phase and the oil phase, and stir and emulsify with a mechanical stirrer at a rotating speed of 1000rmp to obtain such figure 1 The oil-in-water photosensitive particles stabilize the emulsion as shown.

[0041] Preparation of thin-walled hollow spheres:

[0042] (1) Utilize the 500ml deionized water that hydrochloric acid adjusts pH to 4.8 to dilute the above-mentioned obtained emulsion, and stir 5 minutes under the rotating speed of 400rmp with the stirrer, then irr...

Embodiment 2

[0046] Preparation of water-in-oil photosensitive particle stabilized emulsion:

[0047] (1) Water phase: Prepare 30 g of water-based alumina ceramic slurry with a solid phase content of 52 wt%, wherein the average particle size of alumina is 0.5 μm, add 0.14 g of valeric acid, and adjust the pH to 4.6;

[0048] (2) Oil phase: uniformly mix pentaerythritol tetraacrylate and 819 photoinitiators with a total mass of 35g, wherein the quality of 819 photoinitiators is 2wt% of the pentaerythritol tetraacrylate mass;

[0049] (3) Emulsification: Mix the water phase and the oil phase, and stir and emulsify with a mechanical stirrer at a rotational speed of 1000 rpm to obtain a water-in-oil type photosensitive particle stable emulsion.

[0050] Preparation of thin-walled hollow spheres:

[0051] (1) Dilute the emulsion obtained above with 500ml of octane, and stir with a stirrer at a rotating speed of 400rmp for 5 minutes, then irradiate with a single light source of 405nm to trigger...

Embodiment 3

[0055] Preparation of water-in-oil photosensitive particle stabilized emulsion:

[0056] (1) Water phase: prepare 50 g of photosensitive water-based alumina sol slurry with a solid phase content of 30 wt%, and the contents of acrylamide, methylenebisacrylamide and photoinitiator 1173D in the water-based slurry are respectively 13wt%, 1wt%, 1wt% of the total mass of the material, the particle size of the aluminum sol nanoparticles is 30nm; add 0.2g valeric acid to adjust the pH of the water-based photosensitive slurry to 4.2;

[0057] (2) Oil phase: uniformly mix pentaerythritol tetraacrylate and 819 photoinitiators with a total mass of 20g, wherein the quality of 819 photoinitiators is 2wt% of the pentaerythritol tetraacrylate mass;

[0058] (3) Emulsification: Mix the water phase and the oil phase, and stir and emulsify with a mechanical stirrer at a rotating speed of 800 rpm to obtain a water-in-oil type photosensitive particle stable emulsion.

[0059] Preparation of thin-wa...

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Abstract

The invention discloses a preparation method of photosensitive particle stabilizing emulsion as well as a preparation method of a thin-wall hollow sphere, and belongs to the technical field of a porous ceramic material. The photosensitive particle stabilizing emulsion is obtained by mixing and emulsifying oil phase and ceramic powder-containing aqueous phase slurry, wherein at least one of the aqueous phase and the oil phase contains a photosensitive material, and a corresponding photoinitiator is added; the thin-wall hollow sphere is prepared by the steps of diluting photosensitive emulsion and applying an external light field to initiate photosensitive oligomer molecular polymerization reaction to obtain a solidified ceramic granule assembling hollow sphere, separating and sintering; thephotosensitive emulsion prepared by the method can be applied to photocuring 3D printing; the hollow sphere prepared by the method is controllable in structure and is widely applied; and the preparation method provided by the invention has the advantages of simplicity, high efficiency and low cost and is easy in industrial promotion.

Description

technical field [0001] The invention belongs to the technical field of porous ceramic materials, and in particular relates to a preparation method of photosensitive particle stable emulsion and thin-walled hollow spheres. Background technique [0002] The research of foam ceramics with complex shape and fine structure and multi-level porous structure plays an important role in promoting the development of national economy and national defense. Some studies have used direct writing molding technology to print particle-stabilized foam / emulsion ceramics, and the results have confirmed that the hierarchical porous ceramic materials prepared by 3D printing have better comprehensive properties, especially excellent mechanical properties. However, the direct writing molding technology can only prepare ceramic products with relatively simple shapes and specific macroscopic frame structure shapes, and it is still unable to meet the preparation of multi-level porous ceramic materials ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/634C04B35/111C04B35/486C04B35/622B33Y70/00
CPCB33Y70/00C04B35/1115C04B35/486C04B35/622C04B35/63424C04B35/63456C04B2235/3218C04B2235/5436C04B2235/5445C04B2235/5454C04B2235/656C04B2235/94C04B2235/95
Inventor 杨金龙霍文龙张笑妍陈雨谷席小庆王亚利
Owner TSINGHUA UNIV
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