Polymer cross-linking agent based on polyhedral oligomeric silsesquioxane structure

A technology of silsesquioxane and cross-linking agent, which is applied in the direction of silicon organic compounds, can solve the problems of many by-products, cumbersome preparation methods, and low yield, and achieve convenient operation, simple preparation process, and improved cross-linked structure Effect

Pending Publication Date: 2022-05-06
NEW MATERIAL INST OF SHANDONG ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation method used in this patent is relatively cumbersome, including steps such as hydrosilylation addition-hydrolysis condensation-suction filtration-alcohol washing-recrystallization, etc., resulting in many by-products and low yield

Method used

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  • Polymer cross-linking agent based on polyhedral oligomeric silsesquioxane structure
  • Polymer cross-linking agent based on polyhedral oligomeric silsesquioxane structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Preparation of functionalized POSS pre-reaction solution

[0024] Add 40g of toluene to the four-necked flask, slowly add 1g of octahydro-based POSS at room temperature, pass N 2 Protect and stir slowly; after the addition is complete, raise the temperature to 50°C and stir rapidly for 1.5h until the solution is colorless or light yellow and transparent. Naturally cooled to room temperature, 0.00015 g of chloroplatinic acid catalyst was added thereto to obtain a POSS pre-reaction liquid.

[0025] (2) Preparation of POSS-based crosslinking agent

[0026] Mix and dissolve 3g of vinyl silicone oil and 30g of toluene, and slowly add it dropwise to the POSS pre-reaction solution at room temperature. After the addition is complete, N 2 Under protection, the temperature was raised to reflux for 20 h. After the reaction was completed, the catalyst was adsorbed and removed by activated carbon, and the solvent was distilled off under reduced pressure to obtain a light yell...

Embodiment 2

[0028] (1) Preparation of functionalized POSS pre-reaction solution

[0029] Add 40g of toluene to the four-necked flask, slowly add 1g of octahydro-based POSS at room temperature, pass N 2 Protect and stir slowly; after the addition is complete, raise the temperature to 50°C and stir rapidly for 1.5h until the solution is colorless or light yellow and transparent. Naturally cooled to room temperature, 0.0002 g of a chloroplatinic acid catalyst was added thereto to obtain a POSS pre-reaction liquid.

[0030] (2) Preparation of POSS-based crosslinking agent

[0031] Mix and dissolve 1.8g vinyltrimethoxysilane and 20g toluene, slowly add dropwise to the POSS pre-reaction solution at room temperature, after the dropwise addition, N 2 Under protection, the temperature was raised to reflux for 18 hours. After the reaction was completed, the catalyst was adsorbed and removed by activated carbon, and the solvent was distilled off under reduced pressure to obtain a light yellow liq...

Embodiment 3

[0033] (1) Preparation of functionalized POSS pre-reaction solution

[0034] Add 30g of tetrahydrofuran into the four-neck flask, slowly add 1g of octahydroPOSS at room temperature, and pass N 2 Protect and stir slowly; after the addition is complete, raise the temperature to 60°C and stir rapidly for 2 hours until the solution is colorless or light yellow and transparent. Naturally cooled to room temperature, 0.0003 g of chloroplatinic acid catalyst was added thereto to obtain a POSS pre-reaction liquid.

[0035] (2) Preparation of POSS-based crosslinking agent

[0036] Mix and dissolve 1.5g allyl glycidyl ether and 30g tetrahydrofuran, and slowly add it dropwise to the POSS pre-reaction solution at room temperature. After the dropwise addition, N 2 Under protection, the temperature was raised to reflux for 24 hours. After the reaction was completed, the catalyst was adsorbed and removed by active carbon, and the solvent was distilled off under reduced pressure to obtain a...

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Abstract

The invention relates to a polyhedral oligomeric silsesquioxane (POSS) structure-based polymer cross-linking agent, which belongs to the field of polymer cross-linking agents and comprises the following components in parts by weight: 1 part of a functionalized POSS compound, 1-8 parts of a modified compound, 0.0001-0.0006 part of a catalyst and 30-100 parts of a solvent. The preparation method of the polymer cross-linking agent based on the polyhedral oligomeric silsesquioxane structure comprises the following steps: preparation of a functionalized POSS pre-reaction solution and synthesis of a POSS-based cross-linking agent. The cross-linking agent disclosed by the invention takes POSS as a core, contains active groups such as a silicon hydrogen group, a carbon-carbon double bond and an epoxy group, and can be used as a cross-linking or modifying agent of various polymer materials; the cross-linking agent is high in cross-linking activity, a POSS structure can be introduced into a polymer, a three-dimensional network with POSS as a cross-linking core is formed, and the comprehensive performance of a polymer material is remarkably improved; the preparation process is simple, the operation is convenient, the product is safe and environment-friendly, and the industrialization prospect is good.

Description

technical field [0001] The invention belongs to the field of polymer crosslinking agents, in particular to a polymer crosslinking agent based on a cage silsesquioxane structure. Background technique [0002] Cage silsesquioxane (POSS) is a new type of nano-organosilicon material with a unique polyhedral cage structure. The cage skeleton is composed of Si-O bonds, and the Si atoms at the corners of the polyhedron can be connected to different organic functional groups. This special structure endows POSS with unique physical and chemical properties. [0003] There are three main synthetic methods of POSS, namely, hydrolytic condensation method, vertex-capping method, and functional group transformation method. The vertex-capping method is generally used to synthesize monofunctional POSS, and multifunctional POSS is mainly synthesized by hydrolysis condensation method and functional group conversion method. The hydrolysis condensation method is to prepare POSS monomer through...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/44C08G77/38C07F7/21
CPCC08G77/44C08G77/38C07F7/21
Inventor 王峰彭丹牟秋红李金辉张方志张硕
Owner NEW MATERIAL INST OF SHANDONG ACADEMY OF SCI
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