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A kind of organosilicon microsphere with single hole hollow structure and preparation method thereof

A technology of organosilicon microspheres and organosilanes, which is applied in the field of organosilicon microspheres and their preparation, can solve problems such as thermodynamic instability, irregular shape of hollow microspheres, cumbersome preparation process, etc., to avoid surface modification process, The effect of short reaction cycle and simple process

Active Publication Date: 2016-01-27
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because it involves the preparation and removal of the template, the preparation process is cumbersome, and the removal of the template often makes the shape of the hollow microspheres irregular, and the polymer emulsion droplet itself is a thermodynamically unstable system, which makes the hollow microspheres in size Difficult to control size uniformity
In addition, removing the template by high-temperature calcination will decompose the organic groups in the hollow organosilane particles, thus losing the advantages of organic-inorganic hybridization. In order to obtain organic groups, the surface needs to be modified again

Method used

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  • A kind of organosilicon microsphere with single hole hollow structure and preparation method thereof
  • A kind of organosilicon microsphere with single hole hollow structure and preparation method thereof
  • A kind of organosilicon microsphere with single hole hollow structure and preparation method thereof

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Effect test

Embodiment 1

[0032] Embodiment 1, prepare the organosilicon microsphere of single hole hollow structure

[0033] Aminopropyltriethoxysilane and ethyl orthosilicate were mixed and stirred at room temperature for 30 minutes at a material ratio of 4.5:1 to obtain an organosilane mixture; 0.9 grams of the above organosilane mixture was taken dropwise at a speed of 200 rpm Add dropwise to 8 grams of deionized water, raise the temperature to 50°C, keep the speed constant, react for 4 hours, and then age at 50°C for 5 hours; finally centrifuge, wash repeatedly with deionized water, freeze-dry, and the resulting particles The average particle size is 0.75 μm, and the particle size distribution is 0.62 μm to 0.98 μm. After drying, 0.3 grams of organic silicon microspheres are obtained. The total pore area measured by mercury porosimetry is 101.9 m 2 / g, BET specific surface area by nitrogen adsorption method is 47.1m 2 / g, such as figure 1 shown.

Embodiment 2

[0034] Embodiment 2, prepare the organosilicon microsphere of single hole hollow structure

[0035] Aminopropyltriethoxysilane and ethyl orthosilicate were mixed and stirred at room temperature for 30 minutes at a material ratio of 4.5:1 to obtain an organosilane mixture; 0.9 grams of the above organosilane mixture was taken dropwise at a speed of 200 rpm Add it dropwise to 8 grams of deionized water, keep the rotation speed constant at 0°C in an ice-water mixed bath, react for 4 hours, and then age at 0°C for 5 hours; finally centrifuge, wash repeatedly with deionized water, and freeze-dry to form The average particle size of the particles is 2.05 μm, and the particle size distribution is 1.75 μm to 2.38 μm. After drying, 0.3 grams of organic silicon microspheres are obtained. The total pore area measured by mercury porosimetry is 150.9m 2 / g, the BET specific surface area measured by nitrogen adsorption method is 60.1m 2 / g, such as image 3 shown.

Embodiment 3

[0036] Embodiment 3, prepare the organosilicon microsphere of single hole hollow structure

[0037] Aminopropyltrimethoxysilane and vinyltrimethoxysilane were mixed and stirred for 30 minutes at a ratio of 4:1 to obtain an organosilane mixture; 1.2 grams of the above-mentioned organosilane mixture was added dropwise at a speed of 200 rpm 8 grams of deionized water, the reaction temperature is 20 ℃, keep the speed constant, react for 15 hours, then age at 20 ℃ for 10 hours; finally centrifuge, wash repeatedly with deionized water, freeze-dry, the average particle size of the generated particles The particle diameter is 1.52 μm, and the particle size distribution is 1.20 μm to 2.08 μm. After drying, 0.33 grams of organosilicon microspheres are obtained. The total pore area is 200.5 m2 measured by mercury porosimetry. 2 / g, the BET specific surface area measured by nitrogen adsorption method is 80.3m 2 / g.

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Abstract

The invention discloses single-pore hollow-structured organosilicon microspheres and a preparation method thereof. The method comprises the steps that: (1) organosilane and amino-containing organosilane are mixed, such that an organosilane mixture is obtained, wherein the organosilane is at least one of compounds represented by a formula of R1xSi(OR2)y, and the amino-containing organosilane is at least one of compounds represented by a formula of R'1xSi(OR2)y; and (2) the organosilane mixture is added into a solvent for carrying out a hydrolysis condensation reaction, such that a product is obtained; wherein the solvent is water or a mixture of water and an organic solvent. The invention provides the method for preparing the single-pore hollow-structured organosilicon microspheres with amino on the surface, and the organosilicon microspheres prepared with the method. According to the invention, no catalyst is applied, no additional template is involved, the process is simple, condition is mild, and reaction period is short. The obtained organosilicon microspheres have a hollow structure, and through single-holes are on the shells of the hollow microspheres. No surface modification is needed to be carried out upon the particles, and the particles have the reactive active group amino group.

Description

technical field [0001] The invention relates to an organosilicon microsphere and a preparation method thereof, in particular to an organosilicon microsphere with a single-hole hollow structure and a preparation method thereof. Background technique [0002] Polyorganosilane refers to a class of polymers containing silicon in the main chain and at least one organic group on the silicon atom. Because it has an organic-inorganic hybrid structure at the molecular level, it has both the excellent properties of organic materials and inorganic materials. Its inorganic skeleton Si-O-Si structure endows the material with good high and low temperature resistance, weather resistance, aging resistance, hydrophobicity, flame retardancy, insulation and dimensional stability, and the organic group makes the material have better toughness, good processability and Reactivity, etc., make it widely used in electronic packaging materials, heat-resistant materials, and optical conduction. [000...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/06
Inventor 杨晓丽周青竹赵宁张小莉徐坚
Owner INST OF CHEM CHINESE ACAD OF SCI