Polyhydroxyalkylphenyl polysilsesquioxane and preparation method and application thereof

A technology of polysilsesquioxane and polyhydroxyalkyl benzene is applied in the field of polysilsesquioxane POSS and its modified materials, which can solve the problem that the flame retardancy and mechanical properties of polyurethane materials cannot be satisfied at the same time. The flame retardant effect is lasting and stable, the heat resistance and mechanical properties are improved, and the smoke suppression effect is obvious.

Inactive Publication Date: 2017-05-31
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to overcome the deficiencies in the prior art that cannot simultaneously satisfy the flame-retardant properties and mechanical properties of polyurethane materials, the present invention provides a

Method used

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  • Polyhydroxyalkylphenyl polysilsesquioxane and preparation method and application thereof
  • Polyhydroxyalkylphenyl polysilsesquioxane and preparation method and application thereof

Examples

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Embodiment 1

[0042] Example 1 Preparation of Polysilsesquioxane Modified Polyurethane Rigid Foaming Material

[0043] Synthesis of polyhydroxyalkylphenyl polysilsesquioxanes:

[0044] (1) Weigh glycidyl alcohol and 4-aminophenyltriethoxysilane respectively, under nitrogen protection, in an ice-water bath, add 4-aminophenyltriethoxysilane dropwise to glycidyl alcohol, and the mixture React at 20°C for 5 hours, the molar ratio of glycidol to 4-aminophenyltriethoxysilane is 0.5:1;

[0045] (2) Dissolve the product in (1) in a methanol solution, add dropwise an aqueous hydrogen fluoride solution with a mass concentration of 1.5% under stirring conditions, stir at 20°C for 4 hours, and remove water, methanol, and ethanol by distillation under reduced pressure after the reaction is completed. Vacuum drying at 30°C and -0.080MPa for 1 h to obtain polyhydroxyalkylphenyl polysilsesquioxane POSS nanoparticles, wherein the mass ratio of 4-aminophenyltriethoxysilane to methanol is 1:3, 4- The mass r...

Embodiment 2

[0060] Example 2 Preparation of Polysilsesquioxane Modified Polyurethane Rigid Foaming Material

[0061] Synthesis of polyhydroxyalkylphenyl polysilsesquioxanes:

[0062] (1) Weigh glycidyl alcohol and 4-anilinotriethoxysilane respectively, under the protection of nitrogen, in an ice-water bath, add 4-anilinotriethoxysilane dropwise to glycidol, and the mixture will be at 25 Reaction at ℃ for 10h, the molar ratio of glycidol to 4-anilinotriethoxysilane is 2:1;

[0063] (2) Dissolve the product in (1) in a methanol solution, add dropwise a hydrogen fluoride solution with a mass concentration of 3.5% under stirring conditions, stir at 25° C. for 10 h, and remove water, methanol, and ethanol by distillation under reduced pressure after the reaction is completed. Vacuum drying at 40°C and -0.080MPa for 5 hours to obtain polyhydroxyalkylphenylpolysilsesquioxane POSS nanoparticles, wherein the mass ratio of 4-anilinotriethoxysilane to methanol is 1:10, 4-aniline The mass ratio of ...

Embodiment 3

[0080] Example 3 Preparation of Polysilsesquioxane Modified Polyurethane Rigid Foaming Material

[0081] Synthesis of polyhydroxyalkylphenyl polysilsesquioxanes:

[0082] (1) Weigh glycidyl alcohol and 4-anilinotriethoxysilane respectively, under the protection of nitrogen, in an ice-water bath, add 4-anilinotriethoxysilane dropwise to glycidyl alcohol, and the mixture is at 23 Reaction at ℃ for 8h, the molar ratio of glycidol and 4-anilinotriethoxysilane is 1:1;

[0083] (2) Dissolve the product in (1) in a methanol solution, add dropwise a hydrogen fluoride aqueous solution with a mass concentration of 2.0% under stirring conditions, stir for 5 hours at 24°C, and remove water, methanol, and ethanol by distillation under reduced pressure after the reaction is completed. Vacuum drying at 38°C and -0.080MPa for 3 hours to obtain polyhydroxyalkylphenyl polysilsesquioxane POSS nanoparticles, in which the mass ratio of 4-anilinotriethoxysilane to methanol is 1:5,4-aniline The ma...

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Abstract

The invention discloses polyhydroxyalkylphenyl polysilsesquioxane. The polyhydroxyalkylphenyl polysilsesquioxane has the following structures as shown in description, and can be used for preparing a polysilsesquioxane modified polyurethane hard foaming material. The hard foaming material is prepared from A component and B component; the A component comprises organic polyols, the foaming agent, the stabilizing agent, catalyst, crosslinking agent, polyhydroxyalkylphenyl polysilsesquioxane POSS, and flame retardant; the B component comprises polyisocyanates. In the polyurethane material, the polyhydroxyalkylphenyl polysilsesquioxane POSS is added, the polyhydroxyalkyl POSS monomer is reacted with the polyisocyanates to form a carbamate bond, the POSS in rigid structure is crosslinked into a molecular chain of the polyurethane material so as to enhance the mechanical property and the heat resistance of the polyurethane material. The boron inorganic flame retardant and the silicon-containing POSS produce the synergistic fire retardation effect, and a good smoke inhibition effect is formed at the same time. The reaction process is simple, the operation is convenient, and the POSS is suitable for the industrial production. The invention further discloses the preparation of the POSS.

Description

technical field [0001] The invention belongs to polysilsesquioxane POSS and its modified material, in particular to a polyhydroxyphenyl polysilsesquioxane POSS and its polysilsesquioxane modified polyurethane rigid foaming material and its preparation method. Background technique [0002] Polyurethane, or polyurethane, is a general term for macromolecular compounds containing repeated carbamate groups on the main chain. Polyurethane is a polymer compound formed by addition polymerization of organic diisocyanate or polyisocyanate and dihydroxy or polyhydroxy compound. Polyurethane materials are very versatile and can replace rubber, plastic, nylon, etc., and are used in many fields such as construction, transportation, communication cables, aerospace, and electrical appliances. The molecules of pure polyurethane materials are mainly C and H elements, which are extremely flammable, and a flame will be generated immediately when it comes into contact with a fire source, which...

Claims

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Application Information

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IPC IPC(8): C08G77/04C08G77/26C08G18/48C08G18/42C08G18/61C08G18/32C08G18/66C08J9/14C08K3/38
CPCC08G77/045C08G18/3206C08G18/3275C08G18/3281C08G18/4018C08G18/42C08G18/4845C08G18/4854C08G18/61C08G18/6611C08G18/6622C08G18/6655C08J9/141C08J9/144C08J2203/142C08J2205/10C08J2375/04C08J2375/06C08J2375/08C08K3/38C08K2003/387
Inventor 丁寅徐东洋
Owner NANJING UNIV
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