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Method for initiating free radicals of allyl monomer to polymerize by using graphite oxide as initiator

A technology of vinyl monomers and free radicals, which is applied in the field of free radical polymerization, can solve the problems of unaffected ability, weakened and disappeared ability to generate free radicals, and achieve the effect of broad application prospects

Active Publication Date: 2012-08-01
中科金绮新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] A large number of active groups on the surface and between layers of graphite oxide sheets can undergo bond breaking reactions under mild conditions, thereby generating free radicals, but such active functional groups are usually used for surface modification reactions, resulting in its The ability to generate free radicals is significantly weakened or even eliminated, rendering this ability unnoticed

Method used

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  • Method for initiating free radicals of allyl monomer to polymerize by using graphite oxide as initiator
  • Method for initiating free radicals of allyl monomer to polymerize by using graphite oxide as initiator
  • Method for initiating free radicals of allyl monomer to polymerize by using graphite oxide as initiator

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Embodiment 1, graphite oxide initiates the radical polymerization of vinylpyrrolidone (NVP)

[0057] (1) Utilize graphite to prepare graphite oxide with the Hummers method, and its infrared spectrogram is as follows figure 2 shown.

[0058] (2) Get the graphite oxide prepared in 5g step (1), be dispersed in 50g water under mechanical stirring, and pass into N simultaneously 2 For protection, add 10g of NVP (graphite oxide accounts for 50% by mass of NVP) and mix for 30 minutes, then carry out free radical polymerization at 95°C for 30 minutes to obtain vinylpyrrolidone-grafted graphite oxide (PVP-GO).

[0059] The conversion rate of NVP monomer was measured to be 90.1% by weighing method (see the present example for the calculation method).

[0060] The polymer product was diluted with deionized water, separated by suction filtration with a 100nm pore size microporous membrane, the filter cake was refluxed with deionized water for 48 hours, and then placed at 50°C fo...

Embodiment 2

[0069] Embodiment 2, graphite oxide initiates the radical polymerization of methyl methacrylate (MMA)

[0070] (1) Graphite oxide (GO) was prepared by Hummers method using graphite.

[0071] (2) Take 1 g of GO prepared in step (1), disperse it in 100 g of DMSO under mechanical stirring, and feed N 2 Protect, add 500g MMA (graphite oxide accounts for 0.2% by mass percentage of MMA), carry out free radical polymerization at 90°C for 8h, and then heat up to 100°C for free radical polymerization for 6h, use 1 H-NMR measured the molar ratio of MMA monomer / DMSO to calculate the conversion rate of the monomer, and the conversion rate of the monomer was 85%. Dissolve the polymer product obtained above with DMSO, then precipitate and separate with ethanol, filter and separate, and extract the obtained filter cake with ethanol for 48 hours to remove DMSO and MMA monomers, take a part of the filter cake and dry it in vacuum at 50°C for 72 hours to obtain PMMA / GO composite material, an...

Embodiment 3

[0073] Embodiment 3, graphite oxide initiates styrene (St) radical polymerization

[0074] (1) GO was prepared by the Hummers method using graphite.

[0075] (2) Take 1 g of GO prepared in step (1), disperse it in 100 g of DMSO under mechanical stirring, and feed N 2 For protection, add 50g St (graphite oxide accounts for 2% by mass of St), carry out free radical polymerization at 120°C for 8h, use 1 H-NMR measured the molar ratio of styrene monomer / DMSO to calculate the conversion rate of the monomer, and the conversion rate of the monomer was 76%. The polymerization product obtained above was separated by ethanol precipitation, separated by filtration, and the filter cake was first extracted with ethanol for 48 hours to remove DMSO and St monomer, and then extracted with THF for 48 hours to remove physically adsorbed polystyrene PS, and then vacuum-dried at 80°C Graphite oxide (PS-GO) grafted with polystyrene was obtained; the extracted PS was vacuum-dried at 80°C and then...

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Abstract

The invention provides a method for initiating free radicals of an allyl monomer to polymerize by using graphite oxide as an initiator, wherein the allyl monomer can be at least one of the following 1)-9) substances: 1) vinyl pyrrolidone or its derivatives or their salts; 2) acrylamide or its derivatives or their salts; 3) vinylpyridine or its derivatives or their salts; 4) vinyl imidazole or itsderivatives or their salts; 5) acrylic acid (ester ) or its derivatives or their salts; 6) styrene or its derivatives or their salts;; 7) acrylonitrile or its derivatives; 8) organic acid or its derivatives or their salts; and 9) derivatives of ethene. The polymer-grafted graphite oxide (alkene ) prepared by the invention has wide application prospect in the aspects of toughening and strengthening of materials, gas or solvent barrier, electronics electrical materials, electromagnetic shielding, antistatic materials and the like.

Description

technical field [0001] The invention relates to a method in which graphite oxide is used as an initiator to initiate free radical polymerization of vinyl monomers. Background technique [0002] Graphene-a single graphite sheet, which combines the advantages of clay and carbon nanotubes, has increasingly shown important application value as a new type of carbon nanoparticles. The chemical structure of graphene is very similar to that of carbon nanotubes. Ordinary carbon nanotubes can be considered to be curled from single-layer or multi-layer graphene. Graphene has a high specific surface area, and its in-plane Young's modulus and thermal conductivity are as high as 1060GPa and 3000Wm, respectively. -1 K -1 , the in-plane conductivity is comparable to that of carbon nanotubes. Graphene is theoretically a more ideal nanofiller for polymer modification than carbon nanotubes. application prospects. [0003] There are many graphene preparation methods reported in the literat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F292/00C08K9/04C08K3/04C09C1/46C09C3/10
Inventor 冯润财管国虎李春成张栋肖耀南郑柳春
Owner 中科金绮新材料科技有限公司