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Preparation method of super-hydrophobic fluorine-containing organic silicon microspheres

A technology of organosilicon microspheres and superhydrophobicity, which is applied in the field of organosilicon materials, can solve the problems such as the difficulty of preparing superhydrophobic microspheres, and achieve the effects of excellent hydrophobicity, good sphericity, and great application potential

Active Publication Date: 2020-12-15
宁波市大学科技园发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The hydrophobic fluorine-containing silicone microspheres prepared in the above-mentioned prior art all adopt a core-shell structure, that is, fluorine-containing compounds are adsorbed or grafted on the surface of the silicone microspheres, which causes certain friction resistance and durability of the hydrophobic material. However, the hydrophobicity of the microspheres prepared by this method is limited by the number of reactive groups on the surface of the silicone core microspheres, making it difficult to prepare superhydrophobic microspheres

Method used

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  • Preparation method of super-hydrophobic fluorine-containing organic silicon microspheres

Examples

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Embodiment 1

[0025] The preparation method of superhydrophobic fluorine-containing silicone microspheres in this embodiment comprises the following steps:

[0026] (1) Mix 5mL of γ-aminopropyltriethoxysilane and 15mL of methyl perfluorobutyrate thoroughly, blow in nitrogen gas, and reflux at 65°C for 12h;

[0027] (2) After the reaction, add 100mL of absolute ethanol and 100mL of perfluorohexane to separate the liquid, take out the lower layer liquid, and obtain perfluorosilane through vacuum distillation;

[0028] (3) Mix 10mL perfluorosilane, 30mL methyltrimethoxysilane, 20mL ethanol and 160mL water evenly, then add tetramethylammonium hydroxide to adjust the pH value to 8.5, and react at 50°C for 4 hours to obtain superhydrophobic fluorine-containing Silicone microspheres with a particle size of 2.9 μm, such as figure 1 As shown, it can be seen that the superhydrophobic fluorine-containing silicone microspheres prepared in this example have a single particle size, good sphericity, a yi...

Embodiment 2

[0030] The preparation method of superhydrophobic fluorine-containing silicone microspheres in this embodiment comprises the following steps:

[0031] (1) Fully mix 5mL of γ-aminopropyltriethoxysilane and 10mL of methyl perfluorobutyrate, blow in nitrogen gas, and reflux at 65°C for 12h;

[0032] (2) After the reaction, add 100mL of absolute ethanol and 100mL of perfluorohexane to separate the liquid, take out the lower layer liquid, and obtain perfluorosilane through vacuum distillation;

[0033] (3) Mix 10mL perfluorosilane, 30mL methyltrimethoxysilane, 20mL ethanol and 160mL water evenly, then add tetramethylammonium hydroxide to adjust the pH value to 8.5, and react at 50°C for 4 hours to obtain superhydrophobic fluorine-containing Silicone microspheres, the particle size is 3.2 μm, and the yield is 89%.

Embodiment 3

[0035] The preparation method of superhydrophobic fluorine-containing silicone microspheres in this embodiment comprises the following steps:

[0036] (1) Fully mix 5mL of γ-aminopropyltriethoxysilane and 10mL of methyl perfluorobutyrate, blow in nitrogen gas, and reflux at 65°C for 12h;

[0037] (2) After the reaction, add 100mL of absolute ethanol and 100mL of perfluorohexane to separate the liquid, take out the lower layer liquid, and obtain perfluorosilane through vacuum distillation;

[0038] (3) Mix 10mL perfluorosilane, 40mL phenyltrimethoxysilane, 30mL ethanol and 160mL water evenly, then add tetramethylammonium hydroxide to adjust the pH value to 8.5, and react at 50°C for 4 hours to obtain superhydrophobic fluorine-containing Silicone microspheres, the particle size is 3.8 μm, and the yield is 90%.

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Abstract

The invention relates to a preparation method of super-hydrophobic fluorine-containing organosilicon microspheres, which comprises the following steps: (1) fully mixing gamma aminopropyl triethoxysilane and methyl perfluorobutyrate, introducing nitrogen, and carrying out reflux reaction; (2) after the reaction is finished, adding absolute ethyl alcohol and a perfluorinated solvent, performing liquid separation, taking out lower-layer liquid, and performing reduced pressure distillation to obtain perfluorosilane; and (3) uniformly mixing the perfluorosilane obtained in the step (2) with trialkoxysilane, ethanol and water, adding tetramethylammonium hydroxide to adjust the pH value to 8.3-8.7, and reacting at 48-52 DEG C for 3.8-4.2 hours, thereby obtaining the super-hydrophobic fluorine-containing organic silicon microspheres. The siloxane structure and the fluorine-containing groups in the microsphere prepared by the method are bonded in a covalent bond form and are uniformly distributed in the whole microsphere, so that the microsphere with a solid structure is formed, and compared with a core-shell microsphere in the prior art, the microsphere has better friction resistance and durability, and as the number of reactive groups is widely distributed, the material has excellent hydrophobicity.

Description

technical field [0001] The invention relates to the field of organosilicon materials, in particular to a method for preparing superhydrophobic fluorine-containing organosilicon microspheres. Background technique [0002] Silicone microspheres have a three-dimensional cross-linked network structure, showing excellent heat resistance, optical properties, lubricating properties, etc., but their side chains are mostly lipophilic methyl groups or long carbon chain alkyl groups, oil resistance, acid and alkali resistance Poor performance and solvent resistance. Fluorine-containing materials have the advantages of outstanding chemical stability, extremely low surface energy and excellent hydrophobic and oleophobic properties, and are known as "special effect materials". The siloxane structure and fluorine-containing groups are covalently bonded in the microspheres at the same time, which can combine the advantages of organic silicon and fluorine-containing materials, so as to obta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/26C08G77/06
CPCC08G77/26C08G77/06
Inventor 王江波
Owner 宁波市大学科技园发展有限公司
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