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Silicane coupling agent surface grafted modified clay as well as preparation method and use thereof

A silane coupling agent and surface grafting technology, applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., can solve problems such as unstable nanocomposite materials, limited types of terminal functional groups, and poor thermal stability of organoclays , to achieve high thermal stability, improve interfacial interaction, and improve the effect of dispersing ability

Inactive Publication Date: 2008-09-03
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Organoclays modified with organic ammonium salts have poor thermal stability, and their thermal decomposition temperature is generally around 200 °C. When polymer / clay nanocomposites are prepared by melt blending, under the action of high temperature and high shear, the Decomposition and loss can lead to collapse of clay sheets, degradation of polymer molecules and instability of nanocomposite structures
Studies have shown that in organic clay, about 20% of the ammonium salt is adsorbed on the side of the clay, which is the main reason for its poor thermal stability (J.Am.Chem.Soc.1940, 62(6): 1457 ~1464; J.Phys.Chem.1952, 56(6):751~753.)
In addition, the commercial organoammonium salts used for organic modification also limit the functionalization of organoclays due to the limited variety of terminal functional groups.

Method used

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  • Silicane coupling agent surface grafted modified clay as well as preparation method and use thereof
  • Silicane coupling agent surface grafted modified clay as well as preparation method and use thereof
  • Silicane coupling agent surface grafted modified clay as well as preparation method and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Disperse 10g of untreated montmorillonite inorganic clay in 200mL of toluene, stir until uniformly dispersed, and form a stable suspension. Slowly drop 5 mL of dodecyltrimethoxysilane into the suspension, stir mechanically, raise the temperature to 110° C., and reflux for 24 hours. After the reaction, the Buchner funnel was suction-filtered, and the filter cake was washed several times with toluene, dried at 80°C for 24 hours, and ground into powder to obtain a modified clay grafted with dodecyltrimethoxysilane on the surface. The grafting amount of dodecyltrimethoxysilane on the modified clay surface grafted with dodecyltrimethoxysilane was measured by TGA to be 0.26×10 -3 mol / g clay.

Embodiment 2

[0040] Measure 80 mL of absolute ethanol and 20 mL of deionized water, mix them in a beaker, and stir them magnetically; add glacial acetic acid to adjust the pH between 4 and 5, add 10 mL of dodecyltrimethoxysilane, and continue stirring at room temperature for 1 hour. A silane solution was obtained.

[0041] Disperse 10g of untreated montmorillonite inorganic clay in a mixed solvent composed of 90mL of n-butanol and 10mL of deionized water, stir until it is uniformly dispersed to form a stable suspension, and add the silane solution obtained by the above method dropwise into the clay suspension In the middle, heat up to 78°C, add glacial acetic acid, adjust the pH between 4 and 5, stir mechanically, and react for 24 hours. After the reaction was completed, the Buchner funnel was suction-filtered, and the filter cake was washed several times with a mixed solvent of absolute ethanol / deionized water until the pH value of the filtrate was 6-7. Dry at 80°C for 24 hours, grind int...

Embodiment 3

[0043] Measure 180mL of absolute ethanol and 20mL of deionized water, mix them in a beaker, and stir mechanically; add glacial acetic acid to adjust the pH between 4 and 5, add 5mL of dodecyltrimethoxysilane, and continue stirring at room temperature for 1 hour. A silane solution was obtained.

[0044] Disperse 10g of untreated montmorillonite inorganic clay in a mixed solvent composed of 180mL of absolute ethanol and 20mL of deionized water, stir until it is uniformly dispersed to form a stable suspension, add the silane solution obtained by the above method dropwise into the clay to suspend In the liquid, heat up to 78°C, add sodium hydroxide solution, adjust the pH between 9 and 10, stir mechanically, and react for 24 hours. After the reaction was completed, the Buchner funnel was suction-filtered, and the filter cake was washed several times with a mixed solvent of absolute ethanol / deionized water until the pH value of the filtrate was 6-7. Dry at 80°C for 24 hours, grind ...

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Abstract

The invention relates to the clay surface modification, in particular to modified clay with silane coupling agent grafted surface, preparation method and application thereof. The grafting modification of the silane coupling agent with a grafting amount of 0.2-5*10<-3> mol / gram clay is performed in solvent by using reactive hydroxyl group on a clay sheet layer. The inventive modified clay, in which the silane coupling agent is grafted on the clay sheet layer via the covalent bond, has strong thermostability and realizes clay functionalization while improving the clay surface lipophilicity. As the inventive clay has high thermostability and enhanced interaction with polymer, it can be used for the preparation of polymer / clay nanometer composite material to improve the clay dispersibility in the polymeric matrix for stripping and dispersing, thereby improving the performance of the composite material.

Description

technical field [0001] The invention relates to surface modification of clay, in particular to modified clay with surface grafted silane coupling agent and its preparation method and application. Background technique [0002] Clay is a resource-rich mineral. Due to its many advantages such as large interlayer ion exchange capacity, high interlayer charge, large diameter-thickness ratio and specific surface area of ​​the sheet, it is widely used in drilling, casting, catalysis, In the production of cosmetics, pharmaceuticals, paints, etc. Scientists from Japan's Toyota Motor Research Institute have prepared polyamide 6 / clay hybrid materials with nanostructures (Polym. Prepr. 1987, 28 (2): 447-448), and revealed that it has light weight, high The field of polymer / clay nanocomposites has aroused great interest of researchers due to its thermal and excellent barrier properties. Among them, the most studied and most promising clay is montmorillonite. Montmorillonite is a layer...

Claims

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Application Information

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IPC IPC(8): C01B33/40C08K9/06
Inventor 阳明书钱钟钟张世民徐新峰王峰文斌丁艳芬
Owner INST OF CHEM CHINESE ACAD OF SCI
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