Carbon nanotube-modified nano-additive and preparation method and application thereof
A technology of nano-additives and carbon nanotubes, applied in additives, base materials, petroleum industry, etc.
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Embodiment 1
[0028] Step (1) Preparation of multi-walled carbon nanotube-poly 3-ethyl-3-hydroxymethyloxetane (MWCNT-PEHO): 100 mg MWCNT-OH was added to 50 mL CH 2 Cl 2 and 2mL boron trifluoride diethyl ether (BF 3 ·OEt 2 ), sonicate for 20min. Then 20mL of 3-ethyl-3-hydroxymethyloxetane (EHO) was added dropwise into the reaction system through the injection pump over 2h. The reaction mixture was stirred at room temperature for 48 h under the protection of argon, and quenched with ethanol after the reaction. To remove PEHO not bonded to MWCNT-OH, the filtered product was redispersed in ethanol, filtered, washed several times with ethanol, and finally washed with CHCl 3 Wash once. The product was dried under vacuum at 60 °C for 4 h.
[0029] Step (2) Preparation of multi-walled carbon nanotube-polymer phosphate esters (MWCNT-PPEs): 100 mg MWCNT-PEHO, 3.5 mL diphenyl phosphate chloride and 20 mg anhydrous aluminum chloride were added to 50 mL under the protection of argon in toluene. ...
Embodiment 2
[0031] Step (1) is the same as in Example 1.
[0032] Step (2) Preparation of multi-walled carbon nanotube-polymer phosphate esters (MWCNT-PPEs): 100 mg MWCNT-PEHO, 3.5 mL diphenyl phosphate chloride and 20 mg anhydrous magnesium chloride were added to 50 mL toluene under the protection of argon . The reaction mixture was stirred at 110 °C for 15 h. The solvent was removed by filtration and washed three times with toluene. After drying, it was redispersed in deionized water, filtered, washed several times, and finally washed three times with ethanol. Dry overnight at 60°C under vacuum.
Embodiment 3
[0034] Step (1) is the same as in Example 1.
[0035] Step (2) Preparation of multi-walled carbon nanotube-polymer phosphate esters (MWCNT-PPEs): 100 mg MWCNT-PEHO, 3.5 mL diphenyl phosphate chloride and 20 mg anhydrous aluminum trichloride were added to the 50mL of toluene. The reaction mixture was stirred at 90 °C for 15 h. The solvent was removed by filtration and washed three times with toluene. After drying, it was redispersed in deionized water, filtered, washed several times, and finally washed three times with ethanol. Dry overnight at 60°C under vacuum.
[0036] Thermal Stability Evaluation
[0037]Thermal stability was determined by STA449C Jupitersimultaneous TG-DSC. Put the raw material MWCNT-OH in Example 1, the intermediate product MWCNT-PEHO, and the product MWCNT-PPEs 5 mg each into the sample cell. The test temperature is from 20 to 800 °C, and the temperature increase rate is 10 °C / min. Under nitrogen environment Determination. The results are attached...
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