Preparation method of fullerol

Abstract

The invention discloses a preparation method of fullerol. The preparation method comprises the following steps: (1) dissolving fullerene in an organic solvent, wherein the organic solvent is selected from an organic matter which is higher than water in relative density, immiscible with water and can dissolve fullerene; then, respectively putting fullerene C2n which is dissolved in the organic solvent, a hydroxylation reagent aqueous solution with appointed concentration and a phase transfer catalyst into a reactor and layering, wherein a water phase is in the upper layer while the organic solvent in the lower layer; (2) opening a reaction system without isolating air, and after continuously stirring for 10-72 hours at room temperature, stopping reaction; (3) separating liquids, after washing the organic solvent with water, recovering for later use, and recovering the solvent from the water phase to obtain a cured fullerol coarse product; and (4) refining the fullerol coarse product to obtain solid pure fullerol. The synthetic process disclosed by the invention is simple, efficient, convenient to operate and easy for scaled production, and the prepared fullerol shows a good electron paramagnetic spinning property.

Description

technical field [0001] The invention belongs to the field of carbon nanometer materials, and relates to a liquid-phase reaction method for preparing fullerenol. Background technique [0002] Take the "star molecule" C 60 The typical representative fullerene-based carbon nanomaterials are difficult to be directly used in physiological media due to their strong hydrophobicity and poor biocompatibility with organisms, which restricts their biological activity and hinders their application in biomedicine. field applications. Fortunately, fullerene molecules contain a large number of conjugated carbon-carbon double bonds, which can be modified with specific hydrophilic reagents to generate water-soluble derivatives, such as: can react with hydroxylating reagents to generate fullerene polyhydroxy Derivatives, namely fullerenol. This kind of derivative not only has good solubility in water phase, but also retains the unique properties of the original fullerene molecule. At pres...

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Problems solved by technology

[0006] (1) Methods 1, 11, and 12 use solid-phase grinding reactions, and a large amount of solid strong alkali is used in the preparation process, which makes the subsequent purification process time-consuming and laborious and difficult to operate;

[0007] (2) methods 2-8, 13 are all solvent method reactions, and solvent is most often selected for use toluene in the reaction, but it is extremely volatile, uses a large amount of toluene in the preparation technology and easily causes environmental pollution, and its dissolving fullerene ability is lower simultaneously ( Such as: toluene is usually dissolved in the preparation process C 60 The concentration is 1.0, 1.5mg / mL), the batch preparation of fullerenol must use a large amount of toluene as a solvent, which increases the operational difficulty of large-scale production;

[0008] (3) In method 3-7, high-concentration / fuming inorganic strong acids, alkali metal elements or borides need to be used, which requires the reaction to occur under extremely harsh conditions, which will lead to a great potential safety hazard in the preparation process, and will also greatly Increase the operational difficulty and production cost of the preparation process;

[0009] (4) Methods 9, 10, and 11 use fullerene derivatives as raw materials to prepare fullerene alcohols, but the acquisition of the derivatives itself is extremely difficult. Obviously, the production cost of preparing fullerene alcohols in this way is also greatly increased ;

[0011] (6) Although method 2 is currently the most commonly used method, the high-concentration inorganic strong alkali solution (such as: 1g / mL NaOH solution equivalent to about 19mol / L) used in this process increases the difficulty of subsequent purification treatment, At the same time, the preparation process is also divided into two steps. Obviously, this method still has room for improvement.

However, these reports often focus on the application of new hydroxylation reagents, and almost uniformly use toluene as the solvent for dissolving fullerenes, but pay little attention to the influence of other solvents used to dissolve fullerenes in the reaction on the preparation process

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