Method for preparing high water solubility fullerol

A technology for fullerols and fullerenes, applied in the field of preparing highly water-soluble fullerols, can solve the problems of complex post-treatment process, difficult application, unfriendly environment, etc., avoid the introduction of metal ions, shorten the process route, Actionable effect

Active Publication Date: 2012-07-18
BEIJING FUNAKANG BIOTECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the methods for preparing fullerols reported at home and abroad are relatively complicated, and usually introduce inorganic metal ions such as Na and K, which are not easy to remove, which greatly limits its application in the biological field.
In addition, fullererols prepared by traditional methods generally have the problem of a small number of hydroxyl groups, which limits the solubility of fullererols in water and cannot meet the application requirements in the biological field.
[0004] The classic preparation methods of fullerenol mainly include (1) 55°C-60°C in N 2 Under protection, use fuming sulfuric acid on C 60 modified to form C 60 Sulfate derivatives of sulfates, and then hydrolyzed to obtain fullerenols with 10-12 hydroxyl groups. The disadvantage is that the preparation process is complex, requiring protective gas, and the number of hydroxyl groups is small, and the solubility in water is not ideal.
More importantly, the fuming sulfuric acid used

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1, by C 60 Preparation of Highly Water-Soluble Fullerenols

[0033] (a) 120mg C 60 Dissolve in 100mL of toluene, ultrasonic at 150W for 2 hours.

[0034] (b) will O 3 and O 2 Follow O 3 The volume ratio is greater than 1% and mixed into C 60 In the toluene solution, brownish-yellow solids were precipitated on the wall of the bottle, and the color of the solution changed from purple to brown.

[0035] (c) filter out the solid insoluble in toluene (i.e. C 60peroxide), rinsed with toluene until the toluene was colorless, and dried.

[0036] (d) Take 50 mg of the solid obtained in (c) and add 100 mL of 30% H 2 o 2 The solution was heated and stirred for 48 hours at a temperature of 50°C. After the reaction was completed, a light yellow solution was obtained.

[0037] (e) the H in the solution obtained in (d) 2 o 2 Evaporate to dryness to obtain a golden yellow powder, which is highly water-soluble fullerenol. The solubility of this water-soluble ful...

Embodiment 2

[0038] Embodiment 2, by C 70 Preparation of Highly Water-Soluble Fullerenols

[0039] (a) 100mg C 70 Dissolve in 100mL of toluene, ultrasonic at 150W for 2 hours.

[0040] (b) will O 3 and O 2 Follow O 3 The volume ratio is greater than 1% and mixed into C 70 In the toluene solution, a brownish-yellow solid was precipitated on the wall of the bottle, and the color of the solution changed from brownish-red to brownish-yellow.

[0041] (c) filter out the solid insoluble in toluene (i.e. C 70 peroxide), rinsed with toluene until the toluene was colorless, and dried.

[0042] (d) 50 mg of the solid obtained in (c) was added to 120 mL of H 2 o 2 , heated and stirred for 48 hours at a temperature of 50°C. After the reaction was completed, a light yellow solution was obtained.

[0043] (e) the H in the solution obtained in (d) 2 o 2 Evaporate to dryness to obtain golden yellow powder, which is highly water-soluble fullerenol. The solubility of this water-soluble fullere...

Embodiment 3

[0044] Embodiment 3, by C 76 、C 78 、C 84 and embedded structure fullerenes to prepare highly water-soluble fullerenols.

[0045] Dissolve various fullerenes in toluene according to their maximum solubility in toluene, and ultrasonicate at 150W for 2 hours. Other experimental steps are the same as in Example 1.

[0046] by C 76 The solubility of the water-soluble fullerenol prepared is 50-65mg / mL; by C 78 The solubility of the water-soluble fullerenol prepared is 50-65mg / mL; by C 84 The solubility of the prepared water-soluble fullerene is 50-65mg / mL; by the embedded structure fullerene, Sc 3 NC 80 The solubility of the prepared water-soluble fullerenol is 20-40 mg / mL.

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PUM

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Abstract

The invention discloses a simple and convenient method for preparing high water solubility fullerol. The method comprises the steps of: firstly, carrying out an oxidation treatment on fullerene used as a raw material to obtain fullerene peroxide; and performing a reaction on the fullerene peroxide and a hydroxylation reagent with oxidizability to obtain the fullerol. A conventional preparation method of the fullerol is complex in process and poor in solubility, and metal ions are unavoidably introduced in a preparation process, so that the conventional preparation method is high in cost and large in environmental hazard. The method for preparing the fullerol disclosed by the invention is simple in process and good in water solubility, and cannot introduce any metal ions, so that the method for preparing the fullerol is low in cost; and the synthesis route is green and environmental-friendly.

Description

technical field [0001] The invention relates to a method for preparing high water-soluble fullerenol. Background technique [0002] In 1985, Kroto, Curl and Smalley et al. discovered the allotrope of carbon with a special structure-fullerene. Due to its unique structure and physical and chemical properties, fullerenes have received extensive attention in many fields, such as solar cells, semiconductors, catalysts, lubricants, etc. At the same time, fullerenes have also been found to show excellent application prospects in the field of biomedicine. In 1992, Charles N. McEwen of DuPont Company discovered that fullerenes have a super strong ability to absorb and eliminate free radicals, thus for the first time proposed the concept that fullerenes can be used as "free radical sponges". Subsequently, fullerene was used in the cosmetics industry as a new type of material with anti-free radical and anti-aging effects. In 2009, someone carried cisplatin on water-soluble fullerene...

Claims

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Application Information

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IPC IPC(8): C01B31/00C01B32/156
Inventor 王春儒陈曲蒋礼
Owner BEIJING FUNAKANG BIOTECH CO LTD
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