Method for producing fullerene water-soluble derivative and recovering triethanolamine oxide
A technology of amine oxide and triethanol, applied in organic chemistry and other directions, can solve problems such as destroying the structure of fullerene derivatives, and achieve the effects of saving production costs and improving the utilization rate of raw materials
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Embodiment 1 3
[0037] Preparation and recovery of embodiment 1 triethanol amine oxide
[0038] (1) Preparation of triethanolamine oxide
[0039] Measure 5 mL of triethanolamine and 3.3 mL of hydrogen peroxide (molar ratio of triethanolamine:hydrogen peroxide=1:1.1). First add triethanolamine into the three-necked flask, and add 25mL of water to dissolve it. Add 0.258g of trisodium citrate and heat up to 60°C. After reaching 60°C, quickly add hydrogen peroxide, stir, and keep warm for 1h. Raise the temperature to 75-80°C for 3.5h and stir.
[0040] After the reaction was completed, 0.63 g of excess sodium persulfate was added to remove excess hydrogen peroxide, and the mixture was allowed to stand for 2 hours. The reaction solution was subjected to rotary evaporation to remove water, and the solution after rotary evaporation was taken, and after standing for 12 hours, the solution was separated into layers, and the upper yellow oil phase was separated and dried to obtain the final product...
Embodiment 2
[0051] Referring to Example 1, changing the molar ratio of triethanolamine:hydrogen peroxide and keeping other conditions unchanged, triethanolamine oxide was prepared, and separated and recovered in a system containing fullerene derivatives. The specific results are shown in Table 1. It can be seen that when triethanolamine: the mol ratio of hydrogen peroxide is 1:1~2, triethanolamine oxide can obtain more than 90% productive rate, and the recovery rate of final triethanolamine oxide is also It can reach more than 80%, and the purity of the recovered triethanolamine oxide is more than 90%, which can realize the effective recovery and utilization of the triethanolamine oxide.
[0052] The recovery effect of triethanolamine oxide under the different molar ratios of table 1 triethanolamine and hydrogen peroxide
[0053]
Embodiment 3
[0055] Referring to Example 1, changing the volume ratio of precipitant isopropanol and n-hexane, and keeping other conditions unchanged, triethanolamine oxide was separated and recovered in the system containing fullerene derivatives. The specific results are shown in Table 2. It can be seen that when the volume ratio of isopropanol and n-hexane is 7:5, the recovery rate and purity of triethanolamine oxide are the highest, the recovery rate can reach 87%, and the purity can reach 95%, so the solvent of this ratio is preferably used as the precipitant.
[0056] The influence of table 2 different isopropanol, n-hexane volume ratio on triethanol amine oxide recovery rate
[0057]
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