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Method for preparing high-solid-content graphene oxide grafted polyacrylate composite emulsion by using in-situ method

A technology of polyacrylate and high solid content, which is applied in the field of in-situ preparation of high solid content graphene oxide grafted polyacrylate composite emulsion, which can solve the problems of poor dispersion and difficult compounding, and achieve improved breaking strength, The effect of water absorption improvement

Active Publication Date: 2014-12-17
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These two methods are simple and easy to implement, but due to the strong intermolecular force and surface inertness between graphene sheets, its dispersion in organic solvents is not good, and it is difficult to carry out deep compounding with other organic substrates.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Step 1: Preparation of double-bonded graphene oxide:

[0035] In a 100mL three-necked flask, add 0.2 parts of graphene oxide (GO), 25 parts of thionyl chloride (SOCl 2 ) and 0.5 parts of N, N-dimethylformamide (DMF), sonicated for 30 minutes;

[0036] Add a reflux device and blow nitrogen, raise the temperature from room temperature to 50°C, and keep it warm for 24h;

[0037] Cool to room temperature, add 20 parts of N,N-dimethylformamide (DMF), and rotate evaporate at 40°C for 1 h;

[0038] Add 0.10 parts of triethylamine and 0.15 parts of hydroxyethyl acrylate (HEA), stir at room temperature for 6 hours, let stand overnight, and remove the supernatant;

[0039] Add 500 parts of distilled water for suction filtration, wash the solid sample with distilled water, dissolve the obtained black powder in 20 parts of distilled water, add 0.2 parts of sodium dodecyl sulfate (SDS), ultrasonicate for 10 minutes, and freeze-dry to obtain double-bonded graphite oxide alkene;

...

Embodiment 2

[0044] Step 1: Preparation of double bonded graphene oxide:

[0045] In a 100mL three-necked flask, add 0.35 parts of graphene oxide (GO), 32 parts of thionyl chloride (SOCl 2 ) and 0.65 parts of N, N-dimethylformamide (DMF), sonicated for 60 minutes;

[0046] Add a reflux device and blow nitrogen, raise the temperature from room temperature to 65°C, and keep it warm for 36h;

[0047] Cool to room temperature, add 23 parts of N,N-dimethylformamide (DMF), and rotate evaporate at 47°C for 1.5h;

[0048] Add 0.17 parts of triethylamine and 0.22 parts of hydroxyethyl acrylate (HEA), stir at room temperature for 9 hours, let stand overnight, and remove the supernatant;

[0049] Add 500 parts of distilled water for suction filtration, wash the solid sample with distilled water, dissolve the obtained black powder in 35 parts of distilled water, add 0.35 parts of sodium dodecyl sulfate (SDS), ultrasonicate for 25 minutes, and freeze-dry to obtain double-bonded graphite oxide alkene...

Embodiment 3

[0054] Step 1: Preparation of double bonded graphene oxide:

[0055] In a 100 mL three-necked flask, add 0.5 parts of graphene oxide (GO), 40 parts of thionyl chloride (SOCl 2 ) and 0.8 parts of N, N-dimethylformamide (DMF), sonicated for 90 minutes;

[0056] Add a reflux device and blow nitrogen, raise the temperature from room temperature to 80°C, and keep it warm for 48h;

[0057] Cool to room temperature, add 26 parts of N,N-dimethylformamide (DMF), and rotate evaporate at 55°C for 2h;

[0058] Add 0.25 parts of triethylamine and 0.30 parts of hydroxyethyl acrylate (HEA), stir at room temperature for 12 hours, let stand overnight, and remove the supernatant;

[0059] Add 500 parts of distilled water for suction filtration, wash the solid sample with distilled water, dissolve the obtained black powder in 50 parts of distilled water, add 0.5 parts of sodium dodecyl sulfate (SDS), ultrasonicate for 40 minutes, and freeze-dry to obtain double-bonded graphite oxide alkene; ...

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Abstract

The invention relates to a method for preparing a high-solid-content graphene oxide grafted polyacrylate composite emulsion by using an in-situ method. The method comprises the following steps: carrying out ultrasonic treatment on mixed graphene oxide, sulfoxide chloride and N,N-dimethyl formamide; refluxing, raising temperature, carrying out heat preservation and cooling; adding N,N-dimethyl formamide to perform rotary evaporation; adding triethylamine and hydroxyethyl acrylate, and dissolving black powder which is obtained by suction filtration and washing into distilled water; adding sodium lauryl sulfate to carry out ultrasonic treatment, thereby obtaining double-bonded graphene oxide; mixing the double-bonded graphene oxide with sodium lauryl sulfate and distilled water to perform ultrasonic treatment; raising temperature and adding ammonium persulfate and distilled water; and dropwise adding acrylic acid, methyl methacrylate, butyl acrylate and an initiator solution, carrying out heat preservation and discharging. By introducing the double-bonded graphene oxide into the preparation process of the polyacrylate emulsion, the obtained composite emulsion is high in solid content, high in film breaking strength, basically invariable in elongation at break, and high in water absorption rate.

Description

technical field [0001] The invention relates to a preparation method of a polyacrylate emulsion, in particular to a method for preparing a high-solid-content graphene oxide grafted polyacrylate composite emulsion by an in-situ method. Background technique [0002] Graphene is a carbon atom with sp 2 The hybrid orbitals form a hexagonal planar film with a honeycomb lattice, which has good electrical, thermal and mechanical properties, so it is widely used in heat-resistant and flame-retardant materials in polymer substrates, composite conductive films, reinforced fibers, etc. Research. Commonly used polymer-graphene composite methods include solution blending, melting, and in-situ methods. The solution blending method is based on a solution system that can both dissolve the polymer and disperse the graphene, and the polymer and the graphene are compounded to a certain extent through the action of the solvent. No solvent is needed in the melting method, and graphene or mod...

Claims

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Application Information

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IPC IPC(8): C08F292/00C08F220/18C08F220/14C08F220/06C08F2/26
Inventor 高党鸽张文博马建中李聪敏梁双婧
Owner SHAANXI UNIV OF SCI & TECH
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