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Method for preparing fullerene derivative from methylene halide

A technology for fullerene derivatives and dihalomethanes, which is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc. Low energy consumption and the effect of expanding production scale

Inactive Publication Date: 2017-07-28
LESHAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Patent CN 201110142776.3 reports a preparation method of fullerene dimer derivatives, using 1,2-HRC 60 As raw materials, fullerene dimer derivatives are obtained in the oxidation process. Such derivatives are a class of potential fullerene polymer precursors and have unique electronic and optical properties, but their synthesis methods still have costs. higher disadvantage
[0008] The above preparation methods of fullerene and its derivatives all have the disadvantages of high raw material cost and low efficiency, which limit the large-scale application of fullerene and its derivatives

Method used

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  • Method for preparing fullerene derivative from methylene halide
  • Method for preparing fullerene derivative from methylene halide
  • Method for preparing fullerene derivative from methylene halide

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Preparation of Fullerene Derivatives by Ionization of Dichloromethane

[0040]

[0041] S1. Put a magnetic stirring bar in a 100mL round bottom flask, and add 50mL of dichloromethane, then press figure 1 Connect the ionization reaction device as shown;

[0042] S2. Place the reaction device in an oil bath, feed high-purity nitrogen into the reaction system, remove the air in the reaction system, pass condensed water, turn on the oil bath, stir and heat to 55°C, and reflux the dichloromethane;

[0043] S3. When the dichloromethane vapor reaches the ionization reaction chamber, the electric spark detector is turned on, and the generated strong arc is introduced into the ionization reaction chamber through the tungsten wire electrode, and part of the dichloromethane vapor is ionized to generate a large amount of soot;

[0044] S4. The unionized dichloromethane is cooled and the soot and insoluble by-products generated by the washing reaction are filtered out by the san...

Embodiment 2

[0048] Preparation of Fullerene Derivatives by Ionization of Dibromomethane

[0049]

[0050] S1. Put a magnetic stirrer in a 100mL round bottom flask, and add 40mL of methylene bromide, press figure 1 Connect the ionization reaction device as shown;

[0051] S2. Place the reaction device in an oil bath, feed high-purity nitrogen into the reaction system, remove the air in the reaction system, pass condensed water, turn on the oil bath, stir and heat to 110°C, and reflux the methylene bromide.

[0052] S3. When the methylene bromide vapor reaches the ionization reaction chamber, the electric spark detector is turned on, and the generated strong arc is introduced into the ionization reaction chamber through the tungsten wire electrode, and part of the methylene bromide vapor is ionized to generate a large amount of soot.

[0053] S4, the unionized dihalomethane is cooled and the soot and insoluble by-products generated by the washing reaction are filtered out by the sand co...

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Abstract

The invention discloses a method for preparing a fullerene derivative from methylene halide. The method comprises the following steps: putting a magnetic stirrer in a round-bottom flask, adding methylene halide which accounts for 1 / 2 the volume of the round-bottom flask, finishing assembling an ionization reaction device, putting into an oil bath pan, introducing an inert gas, eliminating air, stirring and heating to enable the methylene halide to backflow, introducing water into a spherical condenser pipe to cool at the same time; turning on a high voltage power supply generator when the steam of the methylene halide reaches an ionization reaction chamber, introducing a produced strong electric arc into the ionization reaction chamber, ionizing part of the steam of the methylene halide, discharging the produced gas through an anti-inverse suction bubbler, cooling the methylene halide not ionized, and washing the ash produced in the reaction, filtering and removing insoluble by-products through a sand core, dissolving the product in the methylene halide, and enriching in the flask. The used ionization substance is the methylene halide which is cheap and easy to get; the methylene halide is ionized to directly obtain the fullerene derivative, so that the method is more efficient and cheaper, and the energy consumption is lower.

Description

technical field [0001] The invention relates to the field of chemical preparation, in particular to a method for preparing fullerene derivatives from dihalomethane. Background technique [0002] In the past 20 years, especially after Kratschmer succeeded in macroscopically synthesizing fullerenes by the arc method in 1990, the research on allerenes and their derivatives has developed rapidly, and related research has become a new discipline. At present, fullerene and its derivatives are widely used in cosmetics, lubricants, bioactive materials, solar cells, field effect transistors and other fields. Fullerene and its derivatives have very broad application prospects, and the synthesis of fullerenes with special properties Alkenes are currently one of the most active research areas. [0003] Patent CN200510115405.0 reports a method for preparing fullerenes by bombarding a continuously flowing liquid phase containing aromatics and terpenes with a solid-state laser under the p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/26C07C25/22
CPCC07C17/26C07C25/22
Inventor 田冲陈俏孙国峰聂万丽马克西姆陈刚
Owner LESHAN NORMAL UNIV