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Preparation method of C60 oxide

A technology of hydrogen peroxide and temperature control, applied in the field of carbon nanomaterial oxidation, can solve the problems of easy agglomeration and aggregation, hindering molecular level research and operation, and limiting the application of C60.

Inactive Publication Date: 2016-04-20
江苏昇智环保材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

C in its original state 60 It is a macromolecule composed of carbon atoms, generally insoluble in any solvent, and easily condenses into groups in the solution, which hinders its molecular level research and operation, and greatly limits the C 60 Applications in all aspects

Method used

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  • Preparation method of C60 oxide
  • Preparation method of C60 oxide
  • Preparation method of C60 oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] First add 30mL of concentrated nitric acid into the four-necked bottle, then add 60mL of concentrated sulfuric acid, and mechanically stir in an ice-water bath to obtain a mixed acid at a temperature of 5-10°C. Take 0.5g of C 60 Add it, stir for 10 minutes, the temperature is 5-10°C; gradually add 6g of potassium permanganate slowly, the interval between each addition is 15min, keep the temperature below 10°C in the ice-water bath, and the total reaction time is 3 hours; let off the ice water Heating to 50°C and reacting for 15 hours in total; the reaction mixture was cooled to room temperature, and 100 mL of water was slowly added dropwise to dilute. Pour the sample solution into a beaker to dilute to 300mL, and the temperature of the solution is below 40°C; add 5mL of 30% hydrogen peroxide to the solution, and let it stand for 24 hours, then pour off the supernatant; use an appropriate amount of 5% HCl and pure water to Sample washing. The metal ions are washed away...

Embodiment 2

[0026] First add 30mL of concentrated nitric acid into the four-necked bottle, then add 60mL of concentrated sulfuric acid, and mechanically stir in an ice-water bath to obtain a mixed acid at a temperature of 5-10°C. Take 0.5g of C 60 Add it, stir for 10 minutes, the temperature is 5-10°C; gradually add 6 potassium permanganate slowly, the interval between each addition is 15min, keep the temperature below 10°C in the ice-water bath, and the total reaction time is 3 hours; let off the ice water Heating to 50°C and reacting for 15 hours in total; the reaction mixture was cooled to room temperature, and 100 mL of water was slowly added dropwise to dilute. Pour the sample solution into a beaker to dilute to 300mL, and the temperature of the solution is below 40°C; add 5mL of 30% hydrogen peroxide to the solution, and let it stand for 24 hours, then pour off the supernatant; use an appropriate amount of 5% HCl and pure water to Sample washing. The metal ions are washed away, an...

Embodiment 3

[0030] First add 30mL of concentrated nitric acid into the four-necked bottle, then add 60mL of concentrated sulfuric acid, and mechanically stir in an ice-water bath to obtain a mixed acid at a temperature of 5-10°C. Take 0.5g of C 60 Add it, stir for 10 minutes, the temperature is 5-10°C; gradually add 6 potassium permanganate slowly, the interval between each addition is 15min, keep the temperature below 10°C in the ice-water bath, and the total reaction time is 3 hours; let off the ice water Heating to 50°C and reacting for 15 hours in total; the reaction mixture was cooled to room temperature, and 100 mL of water was slowly added dropwise to dilute. Pour the sample solution into a beaker to dilute to 300mL, and the temperature of the solution is below 40°C; add 5mL of 30% hydrogen peroxide to the solution, and let it stand for 24 hours, then pour off the supernatant; use an appropriate amount of 5% HCl and pure water to Sample washing. The metal ions are washed away, an...

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PUM

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Abstract

The invention discloses a preparation method of C60 oxide. The method comprises the following steps: (1) adding 65% concentrated nitric acid into a reactor, adding 98% concentrated sulfuric acid, stirring in an ice water bath to obtain an acid mixture, and controlling the temperature at 5-10 DEG C; (2) adding C60, stirring, and controlling the temperature at 5-10 DEG C; (3) gradually and slowly adding potassium permanganate in batches (the time interval is 15 minutes), and reacting while keeping the ice water bath temperature at 10 DEG C; (4) discharging the ice water, heating to 50 DEG C, and reacting, wherein the total reaction time is 10-20 hours; (5) cooling the reaction mixture to room temperature, and slowly and dropwisely adding water for dilution, wherein the solution temperature is controlled at 40 DEG C or below; (6) adding oxydol into the solution, standing, and pouring out the supernate; and (7) washing the sample with a proper amount of 5% HCl and pure water to remove metal ions, drying the prepared C60 oxide at 100 DEG C, and storing. By using the acid mixture and potassium permanganate to oxidate C60, the oxidated C60 contains abundant carboxyls, hydroxyls and other oxygen-containing functional groups.

Description

technical field [0001] The invention belongs to the technical field of oxidation of carbon nanomaterials, in particular to a carbon dioxide oxide 60 method of preparation. Background technique [0002] C 60 It is a molecule composed of 60 carbon atoms (substances are generally not composed of atoms), shaped like a football, also known as football ene. Among the wide variety of fullerenes, C 60 The most studied because it is the most stable of them all. Due to its special structure and unique physical and chemical properties, C 60 The research on its compounds has become one of the focuses and hotspots of scientists from all over the world. C 60 Atomic clusters and their derivatives have been involved in many fields such as life chemistry, organic chemistry, material chemistry, inorganic chemistry, polymer science, catalytic chemistry, etc., and can be used in composite materials, building materials, surface coatings, rocket materials, etc. C in its original state 60 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
CPCC01P2002/82
Inventor 张超智李婷袁阳牛孟霄苏艳晓
Owner 江苏昇智环保材料有限公司