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Polyhedral oligomeric silsesquioxane (POSS)-containing alpha-amino triethoxy silane as well as preparation method and application thereof

A technology of aminotriethoxysilane and chloromethyltriethoxysilane, which is applied in the field of organosilicon synthesis, can solve the problems of high cost, complicated chemical method, etc., and achieves great application value, simple separation steps, and reaction temperature. Easy-to-control effects

Active Publication Date: 2021-08-13
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can more uniformly disperse the cage structure of POSS in the polymer, and there is no problem of POSS material crystallization and material phase separation. The above two chemical methods are relatively complicated and costly, and need to be carried out under specific reaction conditions (such as light, heating, precious metal catalyst, etc.)

Method used

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  • Polyhedral oligomeric silsesquioxane (POSS)-containing alpha-amino triethoxy silane as well as preparation method and application thereof
  • Polyhedral oligomeric silsesquioxane (POSS)-containing alpha-amino triethoxy silane as well as preparation method and application thereof
  • Polyhedral oligomeric silsesquioxane (POSS)-containing alpha-amino triethoxy silane as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] Preparation of Chloromethyltriethoxysilane

[0070] Add 36.036g of urea and 150ml of petroleum ether into a 250ml three-neck round-bottom bottle, connect a spherical condenser and two constant pressure dropping funnels to the bottle mouth, and put 27.642g of ethanol (after anhydrous treatment) and 30.000g of chlorine under the protection of nitrogen. Methyltrichlorosilane was added to two constant pressure dropping funnels respectively. Under the protection of nitrogen, heat and stir the mixture of urea and petroleum ether to 65°C, then add ethanol and chloromethyltrichlorosilane synchronously at a rate of 1 drop / second; The reaction was stirred at ℃ for 5h. After the reaction, filter the reaction solution to remove insoluble viscous matter; heat the obtained filtrate to 90°C to remove petroleum ether and ethanol, and recover the obtained petroleum ether and ethanol; heat the remaining liquid to 70°C under a vacuum of 10mmHg , the transparent liquid was distilled off ...

Embodiment 2

[0085] The final product of embodiment 1 is used as the crosslinking agent of room temperature vulcanized silicone rubber

[0086] Take three groups of 3g hydroxy silicone oil with a molecular weight of 3000 (hydroxyl content 0.002mol), add 3ml of toluene respectively and stir evenly, then place them in the mold, mix the hydroxyl group in the hydroxy silicone oil with the α-aminotriethoxysilane containing POSS The molar ratios are 1:1, 1:0.5, 1:0.33 respectively, weigh 2.1g (0.002mol), 1.05g (0.001mol), 0.7g (0.00066mol) 1-(3-(α-N -Methyltriethoxysilyl))propyl heptaisobutyl POSS, put into toluene and dissolve respectively, after dissolving in toluene solvent, add dropwise into hydroxyl silicone oil and stir quickly to mix evenly, at 20 ℃, 45% Cross-linking and curing are carried out under humidity.

[0087] The tack-free time of the cross-linked hybrid system was determined by the finger touch method. The surface dry time of the silicone oil in the 1:1 ratio group was 40 min...

Embodiment 3

[0092] The final product of embodiment 1 is used as reinforcing curing agent to epoxy resin E44 reinforcing curing

[0093] Dissolve 3 groups of 2g epoxy resin E44 in the toluene solvent in the single-necked round bottom flask respectively, add 1.6g, 0.8g, 0.533g of 1-(3-(α-N-methyltriethoxysilyl ))Propyl heptaisobutyl POSS, that is, the molar ratios of epoxy resin E44 and α-aminotriethoxysilane containing POSS are 1:1, 1:0.5, 1:0.333, respectively, and the opening of the single-necked round bottom flask Connect the drying tube at the place, then heat to 100°C under magnetic stirring, and react for 24h. After the reaction, the toluene was removed by vacuum distillation (vacuum degree 80 mmHg, heated to 60° C.), and the residue was a white to pale yellow resinous solid. After sampling the three groups of cross-linked cured substances, perform TGA characterization together with the epoxy resin E44 sample cured by 4-4 diaminodiphenylmethane (ie DDM), and compare their thermal st...

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Abstract

The invention relates to POSS (polyhedral oligomeric silsesquioxane)-containing alpha-amino triethoxy silane and a preparation method and application thereof, and the POSS-containing alpha-amino triethoxy silane has a structure as shown in the following formula I. According to the invention, chloromethyl trichlorosilane, which is a by-product of industrial preparation of dimethyldichlorosilane, is used as a raw material, and a target product with high purity and higher yield is prepared by a simple and mild method; and the prepared POSS-containing alpha-amino triethoxy silane is used as a cross-linking agent or a reinforcing curing agent, and is quickly hydrolyzed and cross-linked with a hydroxyl group under the conditions of no catalyst and room temperature, so that a cage structure of polysilsesquioxane is introduced into the material, and the mechanical property and the thermal stability of the modified material are improved.

Description

technical field [0001] The invention relates to a POSS-containing α-aminotriethoxysilane and a preparation method and application thereof, belonging to the technical field of organosilicon synthesis. Background technique [0002] The crosslinking agent of one-component room temperature vulcanized silicone rubber is a polyfunctional silane compound containing hydrolyzable groups, the general formula is R 4-n Si Y n , wherein n=3 or n=4, R is a carbon functional group, Y is a hydrolyzable group; it plays a role in curing and crosslinking in one-component room temperature vulcanizing silicone rubber. [0003] According to the different small molecules removed during the cross-linking of silicone rubber, the cross-linking reaction of silicone rubber can be roughly divided into decarboxylation type, deketoxime type, dealcoholization type, deamination type, deamidation type, acetone removal type and decarboxylation type. Hydroxylamine type. The small molecules removed in the cr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/388C08G77/26C08L83/04C08L83/08C08L63/02
CPCC08G77/045C08L83/04C08L63/00C08L2201/08C08L83/08
Inventor 贝逸翎宋慈刘雷朱庆增
Owner SHANDONG UNIV
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