Amphiphilic polymer taking polyhedral oligomeric silsesquioxane as core and modified LMHs

A silsesquioxane, amphiphilic technology, applied in the field of inorganic/organic hybrid materials, can solve the problems of poor dispersion, affecting the mechanical properties of materials, etc., to improve compatibility, reduce force, and increase interlayer spacing. Effect

Active 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, due to the size effect, the active groups -OH on the surface of LMHs condense with coordinated water molecules to form hard agglomerates, which have poor dispersion in the composite matrix and affect the mechanical properties of the material.

Method used

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  • Amphiphilic polymer taking polyhedral oligomeric silsesquioxane as core and modified LMHs
  • Amphiphilic polymer taking polyhedral oligomeric silsesquioxane as core and modified LMHs
  • Amphiphilic polymer taking polyhedral oligomeric silsesquioxane as core and modified LMHs

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Example 1 PEG-T 10 Preparation of -COOH

[0062] (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. 4 ;

[0063] (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 cat...

Embodiment 2

[0066] Example 2 PEG-T 10 Preparation of -COOH

[0067] (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. 4 ;

[0068] (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 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 c...

Embodiment 3

[0071] Example 3 PEG-T 10 Preparation of -COOH

[0072] (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. 4 ;

[0073] (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 cata...

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PUM

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Abstract

The invention belongs to the field of inorganic/organic hybrid materials, and discloses an amphiphilic polymer taking polyhedral oligomeric silsesquioxane as a core and modified LMHs. The preparation method comprises the following steps: firstly, preparing an amphiphilic polymer taking polyhedral oligomeric silsesquioxane as a core, and then taking the amphiphilic polymer as an intercalation modifier to react with phenyl carboxylic acid, a metal salt solution and an alkali solution under certain conditions to obtain modified LMHs. The preparation process is simple, the obtained modified LMHs are small in particle size and can be uniformly dispersed in the material, and the thermal stability and the carbon yield of the modified LMHs are improved.

Description

technical field [0001] The invention belongs to the field of inorganic / organic hybrid materials, and specifically relates to an amphiphilic polymer and modified LMHs (Layered metal hydroxides) with cage-shaped silsesquioxane as the core. Background technique [0002] Layered double hydroxides (LDHs) are a class of general formula [M 1-x 2+ m x 3+ (OH) 2 ] X+ [A n- ] x / n ·yH 2 Anionic clays of O, where M 2+ and M 3+ Represent the divalent and trivalent metal cations on the laminate, and the interlayer anion A n- It can vary in a wide range, and the stoichiometric value coefficient X is between 0.2-0.33. Most of the naturally occurring LDHs are magnesium aluminum hydrotalcites, and the interlayer anions are mainly CO 3 2- . According to recent studies, it is more meaningful to design laminates containing LMHs containing three elements of Mg, Al, and Fe in flame retardant materials, because Fe 3+ In the combustion process, it may cause catalysis to form carbon an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G81/00C08G77/392C08L83/07C08L83/05C08K9/06C08K3/22
CPCC08G81/00C08G77/392C08L83/04C08K9/08C08K3/22
Inventor 许凯李东霞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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