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Preparation method of silicon oxide hexatomic ring structural graphene-based polyorganosiloxane

An alkenyl polysiloxane and silicon-oxygen six-membered ring technology is applied in the field of graphene-based polysiloxane materials, which can solve the problems of limited improvement of physical and chemical properties, reduction of comprehensive properties of composite materials, and difficult functionalization of graphene. , to achieve the effect of improving dispersion stability, improving physical and chemical properties, and good dispersion effect

Active Publication Date: 2019-04-23
XINGYE LEATHER TECH CO LTD
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  • Abstract
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  • Claims
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Problems solved by technology

[0004] However, the use of physical blending method to mix graphene or graphene oxide with polysiloxane will have the following problems: (1) graphene has technical defects such as easy agglomeration and reactive inertness, so it is difficult to directly disperse graphene In the polymer system, it is difficult to use graphene to functionalize it. The force between graphene and polysiloxane only exists vander walls force, which does not significantly improve the physical and chemical properties of the material; compared with graphene, oxidation Although graphene can be well dispersed in the polymer system, its physical and chemical properties are significantly lower than that of graphene due to its two-dimensional structure being destroyed; (2) composite mixing is carried out by physical blending method, graphite The combination between ene or graphene oxide and polysiloxane is achieved through van der walls force, and the main chain of polysiloxane is all composed of single bonds, and the Si-O single bond is the most flexible single bond. Therefore, the potential barrier Δμb for the transition between polysiloxane spatial conformations is much smaller than the external field energy, so the polysiloxane monomers are coiled randomly in space, and the polysiloxane chain segments can continuously change their conformations
Since the intermolecular force is far weaker than the covalent bond, the polysiloxane segment is too flexible, and it is difficult to anchor graphene or graphene oxide on the polysiloxane by relying on the van der walls force. As a result, the dispersion of graphene or graphene oxide in polysiloxane is too weak, the improvement of physical and chemical properties is relatively limited, and it is easy to form precipitation or suspension, which greatly reduces the overall performance of the composite material and has low practicability

Method used

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  • Preparation method of silicon oxide hexatomic ring structural graphene-based polyorganosiloxane
  • Preparation method of silicon oxide hexatomic ring structural graphene-based polyorganosiloxane

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Embodiment 1

[0030] A method for preparing graphene-based polysiloxane with six-membered ring structure of silicon oxide includes the following steps:

[0031] Step (1) Graphene oxide modification: Add graphene oxide (single-layer graphene oxide) to the silane coupling agent (3-aminopropyltriethoxysilane), and then add N,N-dicyclohexyl Carbodiimide, the concentration of the graphene oxide in the silane coupling agent is 5g / L, the concentration of the N,N-dicyclohexylcarbodiimide in the silane coupling agent is 5g / L, ultrasonic Disperse for 60min (ultrasonic dispersion power is 120W) to obtain graphene oxide dispersion, transfer it to the reactor and react at 70℃ for 24h, then filter and wash the reaction mixture and vacuum dry (vacuum drying temperature is 50℃, drying time is 48h ) Obtain a solid powder, and obtain modified graphene oxide after reduction (the reduction method is a reduction treatment with a 2% potassium iodide solution for 6 hours);

[0032] Step (2) Preparation of modified po...

Embodiment 2

[0035] A method for preparing graphene-based polysiloxane with a siloxane six-membered ring structure includes the following steps:

[0036] Step (1) Graphene oxide modification: Add graphene oxide (single-layer graphene oxide) to the silane coupling agent (3-chloropropyltriethoxysilane), and graphene oxide in the silane coupling agent The concentration of N,N-dicyclohexylcarbodiimide is 7.5g / L, and then N,N-dicyclohexylcarbodiimide is added. The concentration of N,N-dicyclohexylcarbodiimide in the silane coupling agent is 7.5g / L, ultrasonic Disperse for 90 minutes (ultrasonic dispersion power is 60W) to obtain graphene oxide dispersion, transfer it to the reactor and react at 70°C for 36 hours, and filter the reaction mixture and vacuum dry (vacuum drying temperature is 35°C, drying time is 60h ) To obtain a solid powder, and then to obtain modified graphene oxide after reduction (the reduction method is reduction treatment with a 2.5% hydrazine hydrate solution for 8 hours);

[...

Embodiment 3

[0040] A method for preparing graphene-based polysiloxane with a siloxane six-membered ring structure includes the following steps:

[0041] Step (1) Graphene oxide modification: Add graphene oxide (two-layer graphene oxide) to the silane coupling agent (3-(2,3 glycidoxy)propyltriethoxysilane), and oxidize The concentration of graphene in the silane coupling agent is 7.5g / L, and then N,N-dicyclohexylcarbodiimide is added. The concentration of N,N-dicyclohexylcarbodiimide in the silane coupling agent is 7.5g / L, ultrasonic dispersion for 60min (ultrasonic dispersion power is 150W) to obtain graphene oxide dispersion, transferred to the reactor and reacted at 70 ℃ for 24h, the reaction mixture was filtered, washed and vacuum dried (vacuum drying temperature is 50 ℃, drying time is 48h) to obtain solid powder, after reduction (reduction method is first reduction treatment with 1% potassium iodide solution for 4h, and then reduction treatment with 2% hydrazine hydrate solution for 4h)...

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Abstract

The invention relates to the technical field of graphene-based polyorganosiloxane materials, and provides a preparation method of silicon oxide hexatomic ring structural graphene-based polyorganosiloxane. Graphene oxide is adopted as a raw material, the graphene oxide is modified by the silane coupling agent and then has silane coupling agent modified polyorganosiloxane reaction by using a sol-gelmethod to prepare the silicon oxide hexatomic ring structural graphene-based polyorganosiloxane, so that the dispersion stability of the graphene oxide in the polyorgaonsiloxane can be effectively improved, the advantages of the polyorganosiloxane and graphene are complementary to each other, and a water soluble graphene modified polyorgaonsiloxane material with excellent performance such as electrostaticshielding, high physical performance, high mechanical strength, yellowing resistance and the like.

Description

Technical field [0001] The invention relates to the technical field of graphene-based polysiloxane materials, in particular to a method for preparing graphene-based polysiloxane with a silicon-oxygen six-membered ring structure. Background technique [0002] Polysiloxane has many excellent properties due to its unique structure, and is widely used in many fields such as electronic appliances, automobile transportation, chemical industry, light industry, machinery, construction, and fiber. Polysiloxane is a kind of liquid oil with different viscosity, non-toxic, odorless, non-corrosive and non-flammable. It has a small viscosity-temperature coefficient, high and low temperature resistance, oxidation resistance, high flash point, low volatility, and non-toxic And other characteristics. However, polysiloxane has strong hydrophobicity, which may cause emulsion breaking and sticking to rolls during the use of the product. In addition, traditional polysiloxanes also have defects such ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00
CPCC08G83/001
Inventor 孙辉永姚庆达王小卓梁永贤温会涛周华龙
Owner XINGYE LEATHER TECH CO LTD
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