Method for preparing inorganic crystal whisker/POSS (Polyhedral Oligomeric Silsesquioxane) hybrid material by utilizing sulfydryl-alkene click reaction

A technology of inorganic whiskers and hybrid materials, applied in the direction of coating, etc., to achieve the effects of high grafting efficiency, high yield and mild reaction conditions

Active Publication Date: 2018-07-13
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the method of introducing POSS to the surface of inorgani...

Method used

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  • Method for preparing inorganic crystal whisker/POSS (Polyhedral Oligomeric Silsesquioxane) hybrid material by utilizing sulfydryl-alkene click reaction
  • Method for preparing inorganic crystal whisker/POSS (Polyhedral Oligomeric Silsesquioxane) hybrid material by utilizing sulfydryl-alkene click reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Step 1: Surface mercaptolation of inorganic whiskers

[0043] 0.5g of KH590, deionized water, and absolute ethanol were used to form a mixed solvent with a volume ratio of 1:1:4, and the pH was adjusted to 3-5 with acetic acid, and hydrolyzed at room temperature for 2 hours. 3g basic magnesium sulfate whisker is placed in three-necked flask after ultrasonic dispersion 3min in the mixed solution of absolute ethanol, deionized water (70ml of absolute ethanol, 10ml of deionized water), reflux heating reaction in oil bath. The hydrolyzate was added dropwise, the reaction temperature was controlled at 70° C., and the reaction time was 4 hours. After the reaction, wash with ethanol for 3 to 4 times to remove ungrafted KH590, and dry in a vacuum oven at 70°C for 24 hours to obtain basic magnesium sulfate whiskers with mercaptolation on the surface.

[0044] Step 2: Thiol-ene click reaction

[0045] Dissolve 0.2g of octavinyl POSS and 0.02g of benzoin dimethyl ether in 5ml of...

Embodiment 2

[0048] Step 1: Surface mercaptolation of inorganic whiskers

[0049] 5g of KH590, deionized water, and absolute ethanol were mixed in a volume ratio of 1:1:4, adjusted to pH 3-5 with acetic acid, and hydrolyzed at room temperature for 2 hours. 3g basic magnesium sulfate whisker is placed in three-necked flask after ultrasonic dispersion 3min in the mixed solution of absolute ethanol, deionized water (70ml of absolute ethanol, 10ml of deionized water), reflux heating reaction in oil bath. The hydrolyzate was added dropwise, the reaction temperature was controlled at 70° C., and the reaction time was 4 hours. After the reaction, wash with ethanol for 3 to 4 times to remove ungrafted KH590, and dry in a vacuum oven at 70°C for 24 hours to obtain basic magnesium sulfate whiskers with mercaptolation on the surface.

[0050] Step 2: Thiol-ene click reaction

[0051] Dissolve 0.2g of octavinyl POSS and 0.02g of benzoin dimethyl ether in 5ml of tetrahydrofuran, add 0.5g of mercapto ...

Embodiment 3

[0053] Step 1: Surface mercaptolation of inorganic whiskers

[0054] 0.3g of KH590, deionized water, and absolute ethanol were used to form a mixed solvent with a volume ratio of 1:1:4, and the pH was adjusted to 3-5 with acetic acid, and hydrolyzed at room temperature for 2 hours. 3g basic magnesium sulfate whisker is placed in three-necked flask after ultrasonic dispersion 3min in the mixed solution of absolute ethanol, deionized water (70ml of absolute ethanol, 10ml of deionized water), reflux heating reaction in oil bath. The hydrolyzate was added dropwise, the reaction temperature was controlled at 90°C, and the reaction time was 2h. After the reaction, wash with ethanol for 3 to 4 times to remove ungrafted KH590, and dry in a vacuum oven at 70°C for 24 hours to obtain basic magnesium sulfate whiskers with mercaptolation on the surface.

[0055] Step 2: Thiol-ene click reaction

[0056] Dissolve 0.2g of octavinyl POSS and 0.02g of benzoin dimethyl ether in 5ml of tetrah...

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Abstract

The invention provides a method for preparing an inorganic crystal whisker/POSS (Polyhedral Oligomeric Silsesquioxane) hybrid material by utilizing sulfydryl-alkene click reaction. The method comprises the following steps: under an ultraviolet illumination condition, carrying out the sulfydryl-alkene click reaction by utilizing a double bond (C=C) in vinyl POSS in the presence of sulfydryl (-SH) on the surfaces of inorganic crystal whiskers, so as to combine traditional micron-grade inorganic crystal whiskers with nano-grade POSS, and successfully synthesize the novel inorganic crystal whisker/POSS multi-scale hybrid material. According to the method provided by the invention, the surface performance of the crystal whiskers can be regulated and controlled to the greater extent through adjusting eight organic functional groups on the surface of the POSS, and the surface polarity of the crystal whiskers is improved; compared with an existing traditional crystal whisker surface modification method, the problems of agglomeration of the crystal whiskers and dispersion of the crystal whiskers in organic matrixes can be solved better. The method has the advantages of simple steps, convenience for operation and strong practicability.

Description

technical field [0001] The invention belongs to the technical field of preparation of organic-inorganic hybrid materials, in particular to a method for preparing inorganic whisker / POSS hybrid materials by using mercapto-ene click reaction. Background technique [0002] Inorganic whiskers are fibrous crystals with a certain length-to-diameter ratio. They grow in the form of single crystals and have excellent mechanical properties and chemical stability. They have a wide range of applications in engineering plastics, coatings, heat insulation, and insulating materials. It is called the reinforcing material of the 21st century. However, the particle size of inorganic whiskers is small and the surface energy is high, which makes them prone to agglomeration and bridging during use. Coupled with the strong hydrophilic property of the surface of inorganic whiskers, the compatibility between whiskers and polymer matrix is ​​poor, which limits the popularization and application of w...

Claims

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Application Information

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IPC IPC(8): C08K9/04C08K7/08C09D7/62
CPCC08K7/08C08K9/08
Inventor 张健高传慧任秀刘园园刘月涛张青瑞丁煜武玉民
Owner QINGDAO UNIV OF SCI & TECH
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