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Organosilicon cross-linking agent containing cage oligomeric silsesquioxane structure and preparation method thereof

A technology of polysilsesquioxane and organosilicon crosslinking agent, which is applied in the field of organosilicon crosslinking agent containing cage oligomeric silsesquioxane structure and its preparation, which can solve the problem of poor mechanical properties and adhesive properties and other problems, to achieve the effect of convenient operation, high compatibility and good market prospect

Inactive Publication Date: 2019-02-26
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 shielding effect of side groups makes organopolysiloxane molecules non-polar, and its mechanical properties and adhesive properties are poor when used directly, so it needs to be modified

Method used

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  • Organosilicon cross-linking agent containing cage oligomeric silsesquioxane structure and preparation method thereof
  • Organosilicon cross-linking agent containing cage oligomeric silsesquioxane structure and preparation method thereof
  • Organosilicon cross-linking agent containing cage oligomeric silsesquioxane structure and preparation method thereof

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preparation example Construction

[0039] A method for preparing an organosilicon crosslinking agent containing a cage-type oligomeric silsesquioxane structure. The preparation process steps are as follows, and each component is by weight:

[0040] (1) Preparation of functionalized cage oligomeric silsesquioxane pre-reaction solution:

[0041] Add 20 to 40 parts of the solvent into the reactor, protect it with N2, and slowly add 1 part of functionalized cage-type oligomeric silsesquioxane monomer into the reactor at room temperature, and stir slowly while adding. After the addition is completed, Stir rapidly for 1-2 hours, heat up to 50-60°C, continue to stir until a colorless or light yellow transparent solution; naturally cool to room temperature, add 0.0002-0.0004 parts of catalyst to obtain a functionalized cage oligomeric silsesquioxane pre-reaction solution ;

[0042] (2) Preparation of cage-type oligomeric silsesquioxane-based organosilicon crosslinking agent:

[0043]Mix and dissolve 1 to 5 parts of s...

Embodiment 1

[0047] (1) Preparation of functionalized cage oligomeric silsesquioxane pre-reaction solution

[0048] Add 20g tetrahydrofuran into the four-necked flask, pass N 2 protection, slowly add 1g of octavinyl POSS at room temperature, 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, 0.0002 g of chloroplatinic acid catalyst was added thereto to obtain a pre-reaction liquid.

[0049] (2) Preparation of cage-type oligomeric silsesquioxane-based crosslinking agent

[0050] 1g of phenylhydrogensilane (0.6% hydrogen content) was mixed and dissolved with 20g of tetrahydrofuran, and slowly added dropwise to the cage-type oligomeric silsesquioxane pre-reaction solution at room temperature. 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...

Embodiment 2

[0052] (1) Preparation of functionalized cage oligomeric silsesquioxane pre-reaction solution

[0053] Add 20g tetrahydrofuran into the four-necked flask, pass N 2 protection, slowly add 1g of octavinyl POSS at room temperature, after the addition is complete, raise the temperature to 60°C, and stir rapidly for 2 hours until the solution is light yellow and transparent. Naturally cooled to room temperature, 0.0002 g of chloroplatinic acid catalyst was added thereto to obtain a pre-reaction liquid.

[0054] (2) Preparation of cage-type oligomeric silsesquioxane-based crosslinking agent

[0055] Mix and dissolve 1.2g phenyl hydrogen-containing silicone oil (hydrogen content: 0.5%) and 30g toluene, and slowly add it dropwise to the cage-type oligomeric silsesquioxane pre-reaction solution at room temperature. 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 yel...

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Abstract

The invention relates to an organosilicon cross-linking agent containing a cage oligomeric silsesquioxane structure. The organosilicon cross-linking agent comprises, by weight, 1 part of functionalized cage oligomeric silsesquioxane, 1 to 1 5 parts of silicon hydride, 0.0001 to 0.0004 part of a catalyst and 40 to 90 parts of a solvent. A preparation method for the organosilicon cross-linking agentcontaining the cage oligomeric silsesquioxane structure comprises the synthesis of the cage oligomeric silsesquioxane-based organosilicon cross-linking agent. The organosilicon cross-linking agent ofthe invention contains phenyl groups, has high compatibility with phenyl silicone rubber, and can be used as both a reinforcing filler and a cross-linking agent; the cross-linking agent contains bothhydrosilyl groups and carbon-carbon double bonds, has high cross-linking activity, can form a three-dimensional cross-linking network with POSS as a core, and thus greatly improves the cross-linkingstructure of silicone rubber; and the cross-linking agent of the invention contains both a POSS structure and a benzene ring, and can significantly enhance the mechanical properties and thermal stability of silicone rubber.

Description

technical field [0001] The invention belongs to the field of organosilicon crosslinking agents, in particular to an organosilicon crosslinking agent containing a cage-type oligomeric silsesquioxane structure and a preparation method thereof. Background technique [0002] Cage oligomeric silsesquioxane (POSS) is a nano-organic-inorganic hybrid material with unique physical and chemical properties. The structure is as follows: [0003] [0004] The use of monomers containing POSS structures to modify polymer materials is a current research hotspot. POSS and its derivatives have obtained good results in the fields of polyurethane, epoxy resin, polyimide, polyolefin and other polymer materials. Apply effects. Among them, the multifunctional POSS with high reactivity can be used as a cross-linking component or cross-linking agent to participate in the synthesis and modification of polymers. On the one hand, the POSS structure is introduced into the polymer system, and on the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/44C08G77/04C08L83/10C08L83/04
CPCC08G77/045C08G77/44C08L83/04C08L83/10C08L2201/08C08L2205/02C08L2312/08
Inventor 王峰彭丹牟秋红张方志李冰张硕
Owner NEW MATERIAL INST OF SHANDONG ACADEMY OF SCI
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