CN103274949A - Fullerene ethylenediamine nitrate as well as preparation method and application thereof - Google Patents
Fullerene ethylenediamine nitrate as well as preparation method and application thereof Download PDFInfo
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- CN103274949A CN103274949A CN2013102299390A CN201310229939A CN103274949A CN 103274949 A CN103274949 A CN 103274949A CN 2013102299390 A CN2013102299390 A CN 2013102299390A CN 201310229939 A CN201310229939 A CN 201310229939A CN 103274949 A CN103274949 A CN 103274949A
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- quadrol
- soccerballene
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- nitric acid
- fullerene
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Abstract
The invention discloses a fullerene ethylenediamine nitrate as well as a preparation method and an application thereof. Firstly, fullerene C60 and ethylenediamine are taken as raw materials, fullerene ethylenediamine is prepared by the aid of a nucleophilic addition principle, and the fullerene ethylenediamine reacts with nitric acid so that the fullerene ethylenediamine nitrate is obtained. The fullerene ethylenediamine nitrate has the advantages of oxidant ammonium nitrate (AN), can avoid disadvantages of hygroscopicity, and crystal transformation of AN, and can be used as an oxidant to be applied in a novel solid rocket propellant or explosive.
Description
Technical field
The invention belongs to compound synthetic technical field, be specifically related to soccerballene quadrol nitrate and technology of preparing thereof.This soccerballene quadrol nitrate can be used as solid rocket propellant and fiery explosive oxidizer.
Background technology
Solid propellant is a kind of composite material containing energy with specified property, is the propulsion source of all kinds of solid engines of guided missile, space vehicle.The solid propellant technology is common technology, the support technology of weaponry, also is the restriction technology.Its performance quality directly has influence on viability and the fighting efficiency of Strategy ﹠ Tactics guided missile.
Following tactical missile not only requires solid propellant to have high energy, i.e. high specific impulse, high-density, and require solid propellant on the basis that keeps suitable energy level, have characteristics such as low signature, insensitiveness (low vulnerability) and less contamination.
Ammonium nitrate (AN) propelling agent has advantages such as the combustion temperature is low, the clean no burn into low price of combustion gas is easy to get, but the change of the crystalline substance of ammonium nitrate and moisture-absorption characteristics have troubled the AN propelling agent for many years.
The soccerballene quadrol nitrate of the present invention's preparation can be avoided the shortcoming of ammonium nitrate when having the advantage of ammonium nitrate, be expected to replace the application of ammonium nitrate in solid propellant.
Summary of the invention
One of purpose of the present invention, provide a kind of soccerballene quadrol nitrate that has concurrently in the solid propellant as the richness combustion performance of the oxidisability of the ammonium salt of oxygenant and carbon black, oxygenant used as the rocket engine propelling agent, this material can be avoided shortcomings such as the water absorbability of oxygenant ammonium nitrate and crystal conversion, simultaneously and rich combustible material soccerballene increase the propelling agent specific impulse.Soccerballene and propellant component have good consistency; The crushing resistance of C60 is also fine, and is aging favourable to stoping powder column; The C60 good lubricity can reduce the internal friction that solid propellant adds man-hour simultaneously, increases the compactness of propelling agent.
Two of purpose of the present invention provides the preparation method of above-mentioned substance.
Technical scheme of the present invention is:
Soccerballene quadrol nitrate is characterized in that this structure of matter is suc as formula (1)
In the formula: n≤20 m≤20.
The preparation method of described soccerballene amine metallic salt derivative is raw material with soccerballene C60 and quadrol, obtains the soccerballene sulfonamide derivatives by nucleophilic addition is synthetic, and the soccerballene quadrol makes soccerballene quadrol nitrate with nitric acid reaction again.
The mol ratio of described soccerballene and quadrol is 1:10～1:500, and nitric acid is 1:1～1:40 with the molar mass ratio of soccerballene quadrol.
Concrete preparation method comprises step: at first take by weighing 0.10g C60, add the 50ml quadrol, join in three mouthfuls of round-bottomed flasks of 250ml, under the nitrogen protection, 80 ℃ of reaction 4d become tawny to solution colour, stopped reaction.Down excessive ethylenediamine solution is revolved steaming at 55 ℃-80 ℃ and remove, obtain a large amount of brown dopes.With 4ml dissolved in distilled water dope, add 50ml acetone again, there is a large amount of brown flockss to separate out, filtration under diminished pressure, collecting precipitation gets brown soccerballene quadrol after 45 ℃ of vacuum-dryings.The soccerballene quadrol and the 16ml concentration that take by weighing 1.00g then are the nitric acid of 0.2-15mol/L, temperature control to 0 ℃～90 ℃, stirring reaction 10min～48h.The reaction solution vacuum rotary steam except anhydrating and nitric acid, is got brown solid, and it is that soccerballene quadrol nitrate is product 1 that 45 ℃ of-80 ℃ of vacuum-drying solids obtain the brown solid powder.
Beneficial effect of the present invention:
Soccerballene is the allotropic substance of carbon, be by 60 carbon atoms by the stable especially symmetrical football shaped molecule that big π key system constitutes, have unique physicochemical property.The soccerballene shrink is strong, alleviates water absorbability and the crystal conversion of ammonium nitrate with the nitrate bound energy of quadrol, and during the fullerene ball burning, the specific impulse that can improve propelling agent has good consistency with propellant component; The crushing resistance of C60 is also fine, and is aging favourable to stoping powder column; The C60 good lubricity can reduce the internal friction that solid propellant adds man-hour simultaneously, increases the compactness of propelling agent.
Product preparation mode of the present invention is simple and convenient, separates and purifies easily, and the productive rate height is fit to suitability for industrialized production.
Description of drawings
Fig. 1 is the infrared spectrogram of an example of this soccerballene quadrol nitrate
Fig. 2 is the infrared spectrogram of another example of this soccerballene quadrol nitrate.
Embodiment
The invention will be further described to provide embodiment below; but can not be interpreted as it is limiting the scope of the invention, the person skilled in art must belong to protection scope of the present invention according to the invention described above content to some nonessential improvement and the adjustment that the present invention makes.
Embodiment 1:
At first take by weighing 0.30g C60, add the 200mL quadrol, join in three mouthfuls of round-bottomed flasks of 250mL, under the nitrogen protection, 80 ℃ of reaction 4d become tawny to solution colour, stopped reaction.Down excessive ethylenediamine solution is revolved steaming at 55 ℃ and remove, obtain a large amount of brown dopes.With 8ml dissolved in distilled water dope, add 100 mL acetone again, there is a large amount of brown flockss to separate out, filtration under diminished pressure, collecting precipitation gets brown soccerballene quadrol after 45 ℃ of vacuum-dryings, and its reaction equation is seen formula (2).The soccerballene quadrol and the 16ml concentration that take by weighing 1.00g then are the nitric acid of 1mol/L, temperature control to 40 ℃, stirring reaction 0.5 h.The reaction solution vacuum rotary steam except anhydrating and nitric acid, is got brown solid, and it is that soccerballene quadrol nitrate is product 1 that 45 ℃ of vacuum-drying solids obtain the brown solid powder, its reaction equation is seen formula (3), wherein the m value of product 1 is that 16, n value is 16, its infrared spectrogram such as Fig. 1.
Execute example 2:
At first take by weighing 3.000g C60, add the 1500ml quadrol, join in three mouthfuls of round-bottomed flasks of 2000ml, under the nitrogen protection, 80 ℃ of reaction 4d become tawny to solution colour, stopped reaction.Down excessive ethylenediamine solution is revolved steaming at 55 ℃ and remove, obtain a large amount of brown dopes.With 200ml dissolved in distilled water dope, add 1500 ml acetone again, there is a large amount of brown flockss to separate out, filtration under diminished pressure, collecting precipitation gets brown soccerballene quadrol after 45 ℃ of vacuum-dryings, and its reaction equation is seen formula (4).Taking by weighing 1.00g soccerballene quadrol and 25ml concentration then is the nitric acid of 3mol/L, temperature control to 40 ℃, and stirring reaction 0.5 h, the equation that reacts see formula (5).The reaction solution vacuum rotary steam except anhydrating and nitric acid, is got brown solid, and it is soccerballene quadrol nitrate that 45 ℃ of vacuum-drying solids obtain the brown solid powder, and m value wherein is that 20, n value is 20, its infrared spectrogram such as Fig. 2.
Claims (4)
1. soccerballene quadrol nitrate is raw material with soccerballene C60 and quadrol, utilizes the nucleophilic addition principle to prepare the soccerballene quadrol, and the soccerballene quadrol makes with nitric acid reaction again, its structure as shown in the formula
In under the formula: n≤20 m≤20.
2. the purposes of the described soccerballene quadrol of claim 1 nitrate is used as guided missile rocket engine propelling agent or explosive oxidizer.
3. the preparation method of the described soccerballene quadrol of claim 1 nitrate, it is characterized in that, be raw material with soccerballene C60 and quadrol, obtain the soccerballene quadrol by nucleophilic addition is synthetic, the soccerballene quadrol makes soccerballene quadrol nitrate with nitric acid reaction again;
The mol ratio of described soccerballene and quadrol is 1:10～1:500, and nitric acid is 1:1～1:40 with the molar mass ratio of soccerballene quadrol.
4. as the preparation method of soccerballene quadrol nitrate as described in the claim 3, it is characterized in that the method comprising the steps of:
At first soccerballene and quadrol are put in the reactor, temperature control to 0 ℃～100 ℃, stirring reaction 0.5～20d, after finishing, reaction carries out purification process, that is: revolve steaming earlier and remove excessive quadrol, be dissolved in water, add acetone again and separate out precipitation, the solid that obtains after separation, the drying is the soccerballene quadrol; Taking by weighing a certain amount of red-brown or brownish black soccerballene quadrol and concentration is the 0.2-15mol/L nitric acid reaction, temperature control to 5 ℃～90 ℃, stirring reaction 10min～48 h, get red-brown to dark brown solution, vacuum rotary steam is except anhydrating and nitric acid, and dry back gained solid is the soccerballene quadrol nitrate that makes.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104109457A (en) * | 2014-08-12 | 2014-10-22 | 段小宁 | Preparation method of flame-retardant and waterproof aqueous polyurethane coating and adhesive |
| CN104311427A (en) * | 2014-09-23 | 2015-01-28 | 西南科技大学 | Fullerene poly(glycidyl nitrate), preparation method and application thereof |
| CN104371114A (en) * | 2014-09-23 | 2015-02-25 | 西南科技大学 | Fullerene polyazide glycidyl ether, preparation method and applications thereof |
| CN107555418A (en) * | 2016-06-30 | 2018-01-09 | 中国科学院化学研究所 | Amino fullerene and preparation method thereof |
| CN108324734A (en) * | 2018-02-08 | 2018-07-27 | 中国科学院化学研究所 | Application of the water-soluble fullerenes derivates in enhancing normal cell activity |
| CN109223828A (en) * | 2017-07-11 | 2019-01-18 | 北京福纳康生物技术有限公司 | A kind of amino fullerene is preparing application and anti-biotic material in anti-biotic material |
| CN110041241A (en) * | 2019-05-10 | 2019-07-23 | 西南科技大学 | Fullerene amino benzenes derivates and its preparation method and application |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104109457A (en) * | 2014-08-12 | 2014-10-22 | 段小宁 | Preparation method of flame-retardant and waterproof aqueous polyurethane coating and adhesive |
| CN104109457B (en) * | 2014-08-12 | 2016-03-23 | 段小宁 | A kind of fire-retardant with water-repellancy aqueous polyurethane coating and the preparation method of tackiness agent |
| CN104311427A (en) * | 2014-09-23 | 2015-01-28 | 西南科技大学 | Fullerene poly(glycidyl nitrate), preparation method and application thereof |
| CN104371114A (en) * | 2014-09-23 | 2015-02-25 | 西南科技大学 | Fullerene polyazide glycidyl ether, preparation method and applications thereof |
| CN104311427B (en) * | 2014-09-23 | 2017-02-01 | 西南科技大学 | Fullerene poly(glycidyl nitrate), preparation method and application thereof |
| CN107555418A (en) * | 2016-06-30 | 2018-01-09 | 中国科学院化学研究所 | Amino fullerene and preparation method thereof |
| CN109223828A (en) * | 2017-07-11 | 2019-01-18 | 北京福纳康生物技术有限公司 | A kind of amino fullerene is preparing application and anti-biotic material in anti-biotic material |
| CN108324734A (en) * | 2018-02-08 | 2018-07-27 | 中国科学院化学研究所 | Application of the water-soluble fullerenes derivates in enhancing normal cell activity |
| CN110041241A (en) * | 2019-05-10 | 2019-07-23 | 西南科技大学 | Fullerene amino benzenes derivates and its preparation method and application |
| CN110041241B (en) * | 2019-05-10 | 2022-04-01 | 西南科技大学 | Fullerene aniline derivative and preparation method and application thereof |
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Application publication date: 20130904 |