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Tetraethylene hexaphenyl bifunctional group-containing T10 polyhedral oligomeric silsesquioxane and preparation method thereof

A technology of tetraethylene hexaphenyl bifunctional and vinyl triethoxy siloxane is applied in the field of organic-inorganic nano-hybrid materials, and can solve the problems of low yield, difficulty in separation and purification, low yield of target product and the like, To achieve the effect of simple reaction process, simple post-processing and excellent solubility

Pending Publication Date: 2022-05-31
国科广化精细化工孵化器(南雄)有限公司 +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these synthetic methods cannot control the definite position and exact number of different R groups on the cage molecule, and most of the obtained products are mixed homologues with low yield and difficult separation and purification. Therefore, it is necessary to improve the experimental scheme to obtain specific heterofunctional clathrate silsesquioxane
[0004] At present, cyclotetrasilanol sodium salt is used as the reaction platform, and trichlorosilane is continued to be used for growth on it. The condensation reaction can obtain difunctional cage silsesquioxane, but this scheme is affected by catalysts and experimental conditions that are difficult to control. Low yield of target product

Method used

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  • Tetraethylene hexaphenyl bifunctional group-containing T10 polyhedral oligomeric silsesquioxane and preparation method thereof
  • Tetraethylene hexaphenyl bifunctional group-containing T10 polyhedral oligomeric silsesquioxane and preparation method thereof
  • Tetraethylene hexaphenyl bifunctional group-containing T10 polyhedral oligomeric silsesquioxane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Add 7g CH 3 OK (100mmol) was packed into a 250ml single-necked flask, 90ml of isopropanol was added, 1.8ml of H 2 O (100mmol), the reaction system is white and turbid; 19g (100mmol) vinyltriethoxysilane and 20ml isopropanol that have been added to the constant pressure funnel are slowly added dropwise to the flask, about 10min, and react at room temperature for 24h; continue Add conc. T 4 (as shown in formula I):

[0033]

[0034] (2) The T obtained in step (1) 4 Take 3.5g (10mmol) and 100ml 1,4-dioxane in a 500ml three-necked flask, add 2.3g potassium methoxide and 2g water, stir to dissolve, and pass through N 2 , then slowly add 12.3g (62mmol) of phenyltrimethoxysilane (PTMS) that has been added in the constant pressure funnel into the flask, and at the same time add the catalyst tetramethylammonium fluoride 0.14g (0.146mmol), after the dropwise addition is completed React at 40°C for 24 hours, and then add anhydrous calcium chloride as a catalyst for rem...

Embodiment 2

[0037] (1) Add 7g CH 3 OK (100mmol) was packed into a 250ml single-necked flask, 90ml of isopropanol was added, 1.8ml of H 2 O (100mmol), the reaction system is white and turbid; 19g (100mmol) vinyltriethoxysilane and 20ml isopropanol that have been added to the constant pressure funnel are slowly added dropwise to the flask, about 10min, and react at room temperature for 24h; continue Add conc. T 4 ;

[0038] (2) The T obtained in step (1) 4Take 3.5g (10mmol) and 100ml 1,4-dioxane in a 500ml three-necked flask, add 2.3g potassium methoxide and 2g water, stir to dissolve, and pass through N 2 , then slowly add 14.9g (62mmol) of phenyltriethoxysilane (PTES) that has been added in the constant pressure funnel into the flask, and add catalyst trihydrate tetrabutylammonium fluoride 0.063g (0.2mmol) at the same time, drop After the addition was completed, react at 40°C for 24 hours, and then add anhydrous calcium chloride as a catalyst for removing fluoride ions at room temper...

Embodiment 3

[0040] (1) Add 7g CH 3 OK (100mmol) was packed into a 250ml single-necked flask, 90ml of isopropanol was added, 1.8ml of H 2 O (100mmol), the reaction system is white and turbid; 19g (100mmol) vinyltriethoxysilane and 20ml isopropanol that have been added to the constant pressure funnel are slowly added dropwise to the flask, about 10min, and react at room temperature for 24h; continue Add conc. T 4 ;

[0041] (2) The T obtained in step (1) 4 Take 3.5g (10mmol) and 100ml 1,4-dioxane in a 500ml three-necked flask, add 2.3g potassium methoxide and 2g water, stir to dissolve, and pass through N 2 , then slowly add 15.6g (65mmol) of phenyltriethoxysilane (PTES) that has been added in the constant pressure funnel into the flask, and add the catalyst benzyltrimethylammonium fluoride 0.25g (1.5mmol) at the same time, drop After the completion of the addition, react at 60°C for 24 hours, then add anhydrous calcium chloride as a catalyst for removing fluoride ions at room temperat...

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Abstract

The invention belongs to the technical field of organic and inorganic nano hybrid materials, and discloses T10 polyhedral oligomeric silsesquioxane containing tetraethylene hexaphenyl bifunctional groups and a preparation method of the T10 polyhedral oligomeric silsesquioxane. The preparation method comprises the following steps: dissolving vinyltriethoxysilane in isopropanol, and then adding into a mixed solution containing potassium methoxide and water to obtain tetrahydroxy tetravinyl cyclotetrasiloxane; the preparation method comprises the following steps: dissolving tetraethylene hexaphenyl bifunctional group T10 polyhedral oligomeric silsesquioxane in 1, 4-dioxane, adding phenylsilane and a catalyst, and reacting under the protection of inert gas to obtain the tetraethylene hexaphenyl bifunctional group T10 polyhedral oligomeric silsesquioxane. The method has the advantages of simple reaction process, definite product structure and excellent solubility in common solvents, and can be applied to intercalation modified montmorillonite, hydrotalcite and other inorganic materials to increase the interlayer spacing of the inorganic materials and the like.

Description

technical field [0001] The invention belongs to the technical field of organic-inorganic nano-hybrid materials, and specifically relates to a tetraethylene-hexaphenyl bifunctional group T 10 Cage silsesquioxanes and methods for their preparation. Background technique [0002] Cage-shaped silsesquioxanes (CSQ, Cage-like Silsesquioxanes, also known as polyhedral oligomeric silsesquioxanes) are a type of inorganic skeleton (core) and bonding formed by two-dimensional Si-O-Si short chains. Nano-sized organic-inorganic hybrid closed-type siloxane molecular clusters composed of organic substituents on the cage skeleton, whose general formula is [RSiO 1.5 ] n (n=4, 6, 8, 10, 12, etc.). Among them, n determines its cage topology, which can be abbreviated as T according to different n 6 , T 8 , T 10 etc.; the R group can be an inert group or an active group, and these groups are combined with the vertex silicon atom by a chemical reaction covalent bond to ensure good compatibil...

Claims

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Application Information

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IPC IPC(8): C08G77/20C08G77/06
CPCC08G77/045
Inventor 许凯李东霞刘凌利桂雪峰宋璇王中新林琼林绮欣张天许正敏
Owner 国科广化精细化工孵化器(南雄)有限公司
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