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Multifunctional active POSS (polyhedral oligomeric silsesquioxane), and preparation method and application thereof

A multi-functional and active technology, applied in the field of multi-functional active POSS modified materials, can solve the complex and cumbersome synthesis route of POSS and the mechanical properties of composite polyurethane, and achieve the advantages of easy operation, mild synthesis reaction conditions, enhanced toughness and impact resistance Effect

Inactive Publication Date: 2017-06-13
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to overcome the complex and cumbersome synthesis route of POSS in the prior art, the mechanical properties of composite polyurethane materials and other problems, the present invention provides a synthesis of multifunctional active POSS and its composite polyurethane material

Method used

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  • Multifunctional active POSS (polyhedral oligomeric silsesquioxane), and preparation method and application thereof
  • Multifunctional active POSS (polyhedral oligomeric silsesquioxane), and preparation method and application thereof
  • Multifunctional active POSS (polyhedral oligomeric silsesquioxane), and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Under nitrogen protection, under ice-water bath conditions, 30 g (0.168 mol) of (3-aminopropyl) trimethoxysilane was added dropwise to glycidol solution (24.9 g, 0.336 mol). Carry out ring-opening addition with a reaction time of 8 hours to obtain a trifunctional alkoxy silicone monomer with a polyhydroxy structure; add 120 g of methanol solution to the silanol monomer, and add a hydrogen fluoride aqueous solution with a mass concentration of 1.0% dropwise under stirring conditions. Adjust the pH of the solution to 1.5, carry out hydrolysis and polycondensation at room temperature, and the polycondensation time is 8 hours. After the completion, remove water, methanol and other solvents, and vacuum dry to obtain active POSS with polyhydroxyl groups. Its infrared characteristic peak is: FT-IR (cm -1 ,KBr): 1100(Si-O-Si), 3100(-OH), 1300(C-N), 2850(-CH 2 -).

[0036] Prepare POSS toughening, the raw material formula of reinforced polyurethane foam material is as follows ...

Embodiment 2

[0046] Under nitrogen protection, under ice-water bath conditions, 70.5g (0.3mol) of N-(n-butyl)-aminopropyltrimethoxysilane was added dropwise to glycidyl alcohol solution (7.5g, 0.1mol), and the addition was completed Finally, the ring-opening addition was carried out at room temperature, and the reaction time was 15 hours to obtain a trifunctional alkoxy organosilicon monomer with a polyhydroxy structure; 220 g of methanol solution was added to the silanol monomer, and a mass concentration of 3.5 was added dropwise under stirring conditions. % hydrogen fluoride aqueous solution, adjust the pH of the solution to 3, carry out hydrolysis and polycondensation at room temperature, and the polycondensation time is 24 hours. After the end, remove water, methanol and other solvents, and vacuum dry to obtain active POSS with polyhydroxyl groups. Its infrared characteristic peak is: FT-IR (cm -1 , KBr): 1120 (Si-O-Si), 3200 (-OH), 1290 (C-N), 2850 (-CH 2 -).

[0047] Prepare POSS t...

Embodiment 3

[0059] Under nitrogen protection, under ice-water bath conditions, 44.2 g (0.2 mol) of 4-amino-3,3-dimethylbutyltrimethoxysilane was added dropwise to glycidyl alcohol solution (7.5 g, 0.1 mol). After the addition, ring-opening addition was carried out at room temperature, and the reaction time was 12 hours to obtain a trifunctional alkoxy organosilicon monomer with a polyhydroxy structure; 180 g of methanol solution was added to the silanol monomer, and the mass was added dropwise under stirring. Hydrogen fluoride aqueous solution with a concentration of 2.0%, adjust the pH of the solution to 2, carry out hydrolysis and polycondensation at room temperature, the polycondensation time is 20h, remove water, methanol and other solvents after completion, and vacuum dry to obtain active POSS with polyhydroxyl groups. Its infrared characteristic peak is: FT-IR (cm -1 ,KBr): 1100(Si-O-Si), 3200(-OH), 1320(C-N), 2920(-CH 2 -).

[0060] Prepare POSS toughening, the raw material formu...

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Abstract

The invention relates to a multifunctional active POSS (polyhedral oligomeric silsesquioxane), and application thereof in a hard polyurethane foam material. The multifunctional active POSS has one of the following structures shown below in the specification, wherein the R has one of the following structural formulas shown below in the specification. The multifunctional active POSS has a particle diameter of 2-8 nm, and has favorable compatibility with a polymer material. Under the action of crosslinking with a polyurethane molecular chain, the multifunctional active POSS improves the toughness and shock strength of a polyurethane foam material and enhances the thermal stability of the material to some extent. The invention also discloses a preparation method of the multifunctional active POSS.

Description

technical field [0001] The invention belongs to the field of multifunctional active POSS modified materials, in particular to a multifunctional active POSS and the application of POSS in preparing toughened and reinforced polyurethane foam materials. Background technique [0002] Polysilsesquioxane is a compound with a stable skeleton composed of silicon atoms and oxygen atoms alternately, and its basic structural unit is -Si-O-. Polyhedral cage silsesquioxane (POSS) is a kind of organosilicon compound with special molecular structure, the diameter is between 3-10nm, and the general molecular formula is (RSiO 1.5 ) n , between silica SiO 2 and polysiloxane (R 2 SiO) n Among them, its molecule is based on the inorganic silicon-oxygen skeleton, and the periphery is surrounded by organic groups. The eight Si vertices in the POSS monomer can be connected with organic substituent groups. The inorganic siloxane skeleton endows the material with good heat resistance and mechan...

Claims

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Application Information

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IPC IPC(8): C08G77/04C08G77/06C08G77/16C08G77/26C08G18/61C08G18/48C08J9/14C08G101/00
CPCC08G18/14C08G18/4009C08G18/48C08G18/61C08G77/045C08G77/06C08G77/16C08G77/26C08J9/144C08G2101/00C08J2375/08
Inventor 丁寅徐东洋
Owner NANJING UNIV
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