Preparation and application of amino-functionalized graphene oxide/azo polymer composite waveguide material

Abstract

The invention belongs to the field of polymeric nanocomposite material synthesis, and relates to preparation and application of an amino-functionalized graphene oxide / azo polymer composite waveguide material. The preparation comprises the following steps: firstly preparing azo chromophore 4-(4-nitro-alkenyl)phenyl-1,3-diamine from paranitroaniline and m-phenylenediamine, and then preparing a isocyano-terinated azobenzene prepolymer from NAPD and IPDI in the presence of T-12; afterwards ultrasonically exfoliating graphite oxide to obtain graphene oxide dispersion liquid, and reacting with quadrol under the action of 2-(7-azo benzo triazole)-N, N, N minute, N minute-tetramethyluronium hexafluorophosphate, so as to obtain amino-functionalized graphene oxide; adding the carbimide radical blocked azobenzene prepolymer into EAGO, and performing vacuum drying. A thermo-optical coefficient (dn / dT) of the prepared amino-functionalized graphene oxide / azo polymer composite waveguide material is greater than that of a common organic material and is more than 10 times that of a traditional inorganic material, and the composite waveguide material can be applied to the development of novel digital thermal optical switches with low drive efficiency and higher response speed.

Description

technical field

[0001] The invention belongs to the field of synthesis of polymer nanocomposite materials, and relates to the preparation of functionalized graphene oxide and azo polymer series compounds, in particular to the preparation and application of an amino functionalized graphene oxide / azo polymer composite waveguide material . Background technique

[0002] In recent years, the research hotspots of waveguide optical switches mainly focus on electro-optic switches and thermo-optic switches. Waveguide-type electro-optic switches are fast, but require harsh polarization technology, which is related to polarization and has high cost. For a thermo-optic switch, the thermo-optic effect is used to modulate the light field to realize the switching function. The thermo-optic coefficient of the material is the main factor affecting the driving power and response speed of the thermo-optic switch. Commonly used thermo-optic switch materials are inorganic (such as lithium nioba...

Examples

Embodiment 1

[0027] (1) adopt Hummers method to prepare graphite oxide;

[0028] (2) The azo chromogenic molecule NAPD was prepared by the diazo coupling method;

[0029] (3) Preparation of isocyanate-terminated prepolymer: 1.06 g of NAPD and 2.12 g of IPDI were dissolved in 18.9 g of DMF, and added to a four-neck flask equipped with a stirring bar, a thermometer and a reflux tube. Next, after raising the temperature to 45°C, add 0.5g of T-12 and react for 1 hour to obtain the isocyanate-terminated prepolymer;

[0030] (4) Put 0.012g of graphite oxide in 6gDMF for ultrasonic peeling for 5h, and then centrifuge to obtain a graphene oxide dispersion; place the dispersion in a 250mL round bottom flask, then add 6gEDA into the graphene oxide dispersion, Stir at room temperature for 30 min; then, after heating up to 30°C, add 0.8 mg of 2-(7-azobenzotriazole)-N,N,N',N'-tetramethyluronium hexafluorophosphate ( HATU), continue stirring reaction 3h, obtain the graphene oxide (EAGO) of ethylenedia...

Embodiment 2

[0033] (1) adopt Hummers method to prepare graphite oxide;

[0034] (2) The azo chromogenic molecule NAPD was prepared by the diazo coupling method;

[0035] (3) Preparation of isocyanate-terminated prepolymer: 1.06g of NAPD and 2.12g of IPDI were dissolved in 21.2g of DMF, and added to a four-neck flask equipped with a stirring bar, a thermometer and a reflux tube. Next, after raising the temperature to 50°C, add 0.5g T-12 and react for 2 hours to obtain the isocyanate-terminated prepolymer;

[0036] (4) Put 0.012g of graphite oxide in 7.2g of DMF for ultrasonic peeling for 6h, then centrifuge to obtain the graphene oxide dispersion, put the dispersion in a 250mL round bottom flask, and then add 8.4g of EDA to the graphene oxide dispersion , stirring at room temperature for 30 min; then, after heating up to 40 ° C, adding 0.8 mg HATU, and continuing to stir for 4 h to obtain ethylenediamine-functionalized graphene oxide (EAGO);

[0037] (5) Then add the isocyanate-terminate...

Embodiment 3

[0039] (1) adopt Hummers method to prepare graphite oxide;

[0040] (2) The azo chromogenic molecule NAPD was prepared by the diazo coupling method;

[0041] (3) Preparation of isocyanate-terminated prepolymer: 1.06 g of NAPD and 3.71 g of IPDI were dissolved in 19.08 g of DMF, and added to a four-neck flask equipped with a stirring bar, a thermometer and a reflux tube. Next, after raising the temperature to 80°C, add 0.5g T-12 and react for 4 hours to obtain the isocyanate-terminated prepolymer;

[0042] (4) Put 0.012g of graphite oxide in 9.42g of DMF for ultrasonic peeling for 6h, then centrifuge to obtain the graphene oxide dispersion, put the dispersion in a 250mL round bottom flask, and then add 9g of EDA to the graphene oxide dispersion , stirred at room temperature for 30 min. Next, after raising the temperature to 60°C, add 1 mg HATU, and continue stirring for 6 hours to obtain ethylenediamine-functionalized graphene oxide (EAGO);

[0043] (5) Then, add the isocyan...

technical field

[0001] The invention belongs to the field of synthesis of polymer nanocomposite materials, and relates to the preparation of functionalized graphene oxide and azo polymer series compounds, in particular to the preparation and application of an amino functionalized graphene oxide / azo polymer composite waveguide material . Background technique

[0002] In recent years, the research hotspots of waveguide optical switches mainly focus on electro-optic switches and thermo-optic switches. Waveguide-type electro-optic switches are fast, but require harsh polarization technology, which is related to polarization and has high cost. For a thermo-optic switch, the thermo-optic effect is used to modulate the light field to realize the switching function. The thermo-optic coefficient of the material is the main factor affecting the driving power and response speed of the thermo-optic switch. Commonly used thermo-optic switch materials are inorganic (such as lithium nioba...

Examples

Embodiment 1

[0027] (1) adopt Hummers method to prepare graphite oxide;

[0028] (2) The azo chromogenic molecule NAPD was prepared by the diazo coupling method;

[0029] (3) Preparation of isocyanate-terminated prepolymer: 1.06 g of NAPD and 2.12 g of IPDI were dissolved in 18.9 g of DMF, and added to a four-neck flask equipped with a stirring bar, a thermometer and a reflux tube. Next, after raising the temperature to 45°C, add 0.5g of T-12 and react for 1 hour to obtain the isocyanate-terminated prepolymer;

[0030] (4) Put 0.012g of graphite oxide in 6gDMF for ultrasonic peeling for 5h, and then centrifuge to obtain a graphene oxide dispersion; place the dispersion in a 250mL round bottom flask, then add 6gEDA into the graphene oxide dispersion, Stir at room temperature for 30 min; then, after heating up to 30°C, add 0.8 mg of 2-(7-azobenzotriazole)-N,N,N',N'-tetramethyluronium hexafluorophosphate ( HATU), continue stirring reaction 3h, obtain the graphene oxide (EAGO) of ethylenedia...

Embodiment 2

[0033] (1) adopt Hummers method to prepare graphite oxide;

[0034] (2) The azo chromogenic molecule NAPD was prepared by the diazo coupling method;

[0035] (3) Preparation of isocyanate-terminated prepolymer: 1.06g of NAPD and 2.12g of IPDI were dissolved in 21.2g of DMF, and added to a four-neck flask equipped with a stirring bar, a thermometer and a reflux tube. Next, after raising the temperature to 50°C, add 0.5g T-12 and react for 2 hours to obtain the isocyanate-terminated prepolymer;

[0036] (4) Put 0.012g of graphite oxide in 7.2g of DMF for ultrasonic peeling for 6h, then centrifuge to obtain the graphene oxide dispersion, put the dispersion in a 250mL round bottom flask, and then add 8.4g of EDA to the graphene oxide dispersion , stirring at room temperature for 30 min; then, after heating up to 40 ° C, adding 0.8 mg HATU, and continuing to stir for 4 h to obtain ethylenediamine-functionalized graphene oxide (EAGO);

[0037] (5) Then add the isocyanate-terminate...

Embodiment 3

[0039] (1) adopt Hummers method to prepare graphite oxide;

[0040] (2) The azo chromogenic molecule NAPD was prepared by the diazo coupling method;

[0041] (3) Preparation of isocyanate-terminated prepolymer: 1.06 g of NAPD and 3.71 g of IPDI were dissolved in 19.08 g of DMF, and added to a four-neck flask equipped with a stirring bar, a thermometer and a reflux tube. Next, after raising the temperature to 80°C, add 0.5g T-12 and react for 4 hours to obtain the isocyanate-terminated prepolymer;

[0042] (4) Put 0.012g of graphite oxide in 9.42g of DMF for ultrasonic peeling for 6h, then centrifuge to obtain the graphene oxide dispersion, put the dispersion in a 250mL round bottom flask, and then add 9g of EDA to the graphene oxide dispersion , stirred at room temperature for 30 min. Next, after raising the temperature to 60°C, add 1 mg HATU, and continue stirring for 6 hours to obtain ethylenediamine-functionalized graphene oxide (EAGO);

[0043] (5) Then, add the isocyan...

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