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Method for preparing ethyl nitrofullerene derivative

A technology for nitrofullerene and derivatives, which is applied in attack equipment, nitrification explosive components, organic chemistry, etc., can solve problems such as harsh reaction conditions and poor stability of fullerene nitro compounds.

Inactive Publication Date: 2008-02-13
彭汝芳 +4
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

C 60 React with mercuric nitrate nitrating agents and halogen catalysts at 70-150°C to obtain fullerene nitro compounds (patent number: CN 1884054A); Taiwan's L.Y.Chiang et al. 60 React with concentrated sulfuric acid and potassium nitrate at 95°C to obtain fullerene nitro compounds; F.Cataldo in Italy also tried to nitrate C60 with dinitrogen tetroxide or fuming nitric acid; these methods directly nitrate C60 , the reaction conditions are relatively harsh, and the stability of the obtained fullerene nitro compounds is not very good

Method used

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  • Method for preparing ethyl nitrofullerene derivative
  • Method for preparing ethyl nitrofullerene derivative
  • Method for preparing ethyl nitrofullerene derivative

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Embodiment Construction

[0020] 21.0 mg of 2-(3-nitrophenyl)pyrrolidine[3',4':1,2][60]fullerene, 37.2 mg of 2,4-dinitrofluorobenzene, 32.6 mg of TBAB and 28.0 mg K 2 CO 3 Mix in a 25ml round-bottom flask, ultrasonically sonicate for 10 minutes to mix evenly, place in a constant temperature oil bath at 150°C for 12 hours, cool with a small amount of CS 2 Dissolve the residue, and then use a silica gel column to separate and wash off the product with a brown band using a mixture of n-hexane / toluene with a volume ratio of 1:2 as the eluent.

[0021] The resulting brown product solution was spin-dried, treated with a small amount of petroleum ether and acetone for impurity removal, and vacuum-dried at 60° C. for 10 hours to finally obtain 15.5 mg of a dark brown solid product (yield 22.1%).

[0022] Using FT-IR, MS, 1 The structure of the product was characterized by spectral means such as H NMR and UV-vis.

[0023] As shown in Figure 1, at 527.0, 574.0 and 1187.3cm -1 The absorption peak at C 60 Ch...

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Abstract

The invention uses the indirect method with the nitrogen substituted fullerene pyrrolidine derivative and the nitro-halide benzene as the raw material; under the condition of the phase-transfer catalyst and weak alkali, the solid phase is heated to synthesize a nitryl fullerene derivative; the initial exploration has been done on the stability of the nitryl fullerene derivative so as to acquire an insensitive additive which not only has the energy insensitivity but also has the certain energy contribution; the insensitive additive can be used in the materials containing the energy such as the explosive, propellant, fire supplies and so on.

Description

technical field [0001] The invention relates to nitrofullerene derivatives used as explosive desensitizers and solid rocket propellant additives and a preparation method thereof. Background technique [0002] The research on the insensitivity of explosives has been widely concerned by scholars at home and abroad. Graphite has a layered structure and is often used as an insensitivity agent in explosives. Adding a certain amount of graphite in explosives can reduce the friction between explosive particles and between explosives and surrounding media under the action of external force, resulting in uniform distribution of stress in explosives and making friction The heat generated is concentrated in the graphite layer, reducing the possibility of hot spots, but graphite does not contribute energy to the explosive. Therefore, it is of scientific significance and application value to seek an energetic desensitizing agent that can not only desensitize but also contribute certain ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/56C06B25/00
Inventor 彭汝芳黄毅民楚士晋徐瑞娟金波
Owner 彭汝芳
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