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Graphene/polysiloxane spun fiber membrane and preparation method thereof

A technology of polysiloxane spinning and polysiloxane is applied in the field of graphene/polysiloxane spinning fiber film and its preparation, and can solve the problem of difficult fibers, low crystallinity, and secondary valence between polymer chains. problems such as small force, to achieve the effects of mild reaction conditions, simple preparation method and controllable pore size

Active Publication Date: 2021-10-22
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention does not clarify the molecular structure of the vinyl polysiloxane material. If the polymer is a linear polysiloxane with a weight average molecular weight in the range of 5,000-180,000 g / mol, the polymer is fluid or highly viscous Fluid, electrospinning can not get a formed fiber membrane structure; if it is cross-linked vinyl polysiloxane, the inventive method cannot make a good spinning solution, so it is impossible to obtain a fiber membrane with good shape and other properties
[0003] Linear polysiloxanes are usually viscous fluids with small secondary valence forces between polymer chains and low crystallinity, making it difficult to prepare fibers with good mechanical properties by traditional methods; while cross-linked polysiloxanes usually cannot obtain good Therefore, it is impossible to obtain fiber membranes with good morphology and other properties by electrospinning.

Method used

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  • Graphene/polysiloxane spun fiber membrane and preparation method thereof
  • Graphene/polysiloxane spun fiber membrane and preparation method thereof
  • Graphene/polysiloxane spun fiber membrane and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0042] A kind of preparation method of graphene / polysiloxane spinning fiber film, comprises steps:

[0043] Add 5.0g graphene to 10.0mL tetrahydrofuran solution of methyltrimethoxysilane with a concentration of 5mg / mL, ultrasonically disperse and mix evenly, then stir and react at 50°C for 24.0h to obtain a graphene suspension; add 160.0g formazan Dimethyldiethoxysilane and 10.0g dimethyldiethoxysilane were mixed evenly, and the graphene oxide suspension prepared above was added, ultrasonically dispersed, stirred until a uniform dispersion was formed, and the weight percentage concentration was 10.0wt%. dilute hydrochloric acid aqueous solution until the reactant system pH = 3.0. React at 80°C for 6h, then decompress and remove the low molecular weight for 1.0h at a vacuum of 10mmHg and a temperature of 90°C to obtain a polysiloxane prepolymer (liquid resin); by controlling the above polycondensation reaction conditions and decompression decompression In addition to low molec...

Embodiment 2

[0046] A kind of preparation method of graphene / polysiloxane spinning fiber film, comprises steps:

[0047] Add 35.0 g of graphene to 40.0 mL of phenyltrimethoxysilane toluene solution with a concentration of 15 mg / mL, ultrasonically disperse and mix evenly, and then stir and react at 60° C. for 30.0 h to obtain a graphene suspension. Mix 140.0g of phenyltrimethoxysilane with 100.5g of γ-mercaptopropylmethyldiethoxysilane evenly, add the graphene oxide suspension prepared above, ultrasonically disperse, stir rapidly until a uniform dispersion is formed, add weight Dilute hydrochloric acid aqueous solution with a percentage concentration of 10.0 wt%, until the pH of the reactant system is 2.0. React at 60°C for 12.0h, then remove low molecules under reduced pressure for 1.2h at a vacuum of 10mmHg and a temperature of 110°C to obtain a polysiloxane prepolymer (liquid resin). Using toluene as a solvent, the prepolymer was formulated into a prepolymer spinning solution with a con...

experiment example 3

[0049] A kind of preparation method of graphene / polysiloxane spinning fiber film, comprises steps:

[0050] Add 15.0 g of graphene to 20.0 mL of methyltriethoxysilane tetrahydrofuran solution with a concentration of 10 mg / mL, ultrasonically disperse and mix evenly, and then stir and react at 40° C. for 30.0 h to obtain a graphene suspension. Mix 105.0g of methyltrimethoxysilane and 50.0g of γ-chloropropylmethyldiethoxysilane evenly, add the graphene oxide suspension prepared above, ultrasonically disperse, stir rapidly until a uniform dispersion is formed, add dilute hydrochloric acid aqueous solution with a weight percent concentration of 10.0wt%, until the reactant system pH=4.0. React at 50°C for 8.0h, then remove low molecular weight under reduced pressure for 1.5h at a vacuum of 10mmHg and a temperature of 95°C to obtain a polysiloxane prepolymer (liquid resin). Using tetrahydrofuran as a solvent, the prepolymer was formulated into a prepolymer spinning solution with a c...

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Abstract

The invention provides a graphene / polysiloxane spun fiber membrane and a preparation method thereof. The preparation method comprises the following steps of dispersing graphene in a silane dilute solution, and performing a stirring reaction to obtain a graphene suspension; uniformly mixing graphene turbid liquid with a multifunctional silane monomer, adding a catalyst, performing a hydrolysis pre-polycondensation reaction, and removing small molecules under reduced pressure to prepare a prepolymer; dissolving the prepolymer in an organic solvent to prepare a polymer spinning solution; and carrying out electrostatic spinning. According to the preparation method, the polycondensation degree, the crosslinking degree and the structure of the polysiloxane prepolymer for spinning are regulated and controlled, a polysiloxane sol-gel chemical process in a short time of electrostatic spinning is accurately controlled, and graphene is supplemented for supporting and enhancing the fiber performance, so that the graphene / polysiloxane spun fiber membrane is prepared, and the technical difficulty of curing forming of polysiloxane spun fiber is overcome. The prepared fiber membrane has important application prospects in the fields of electrochemistry, catalysis, sensors, adsorption and separation, flexible electronic elements and medical engineering.

Description

technical field [0001] The invention relates to a graphene / polysiloxane spinning fiber membrane and a preparation method thereof, belonging to the technical field of new materials. Background technique [0002] Fibers with good mechanical properties made from polymers by spinning require polymers to be linear polymers with appropriate relative molecular weights, and there must be sufficient secondary valence forces and good crystallization capabilities between molecular chains of polymers. Such as polyethylene terephthalate, polycaprolactam, polyhexamethylene adipamide, polyparaphenylene terephthalamide, polyacrylonitrile and polypyrrolidone. Polysiloxane is a type of polymer with a Si-O-Si main chain structure and one or two organic groups on the silicon atom. It has the characteristics of high and low temperature resistance, weather resistance, hydrolytic stability and biocompatibility. . Chinese patent document CN104805598A discloses a method for preparing a vinyl polys...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D04H1/728D04H1/4242D04H1/4282D01D5/00D01F8/18D01F8/16
CPCD04H1/728D04H1/4242D04H1/4282D01D5/003D01D5/0053D01D5/0061D01F8/18D01F8/16D10B2101/122D10B2401/062
Inventor 朱庆增张蒙蒙
Owner SHANDONG UNIV
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