Fullerene polyglycidyl ether nitrate and preparation method and application thereof

Abstract

The invention relates to fullerene poly(glycidyl nitrate), a preparation method and an application thereof, wherein the fullerene poly(glycidyl nitrate) has the chemical structure formula represented by a formula (I). The invention further relates to the preparation method, which comprises: adopting monomethyl-terminated poly(glycidyl nitrate) (PGN) and malonyl chloride as raw materials, carrying out the esterification and bromination two-step reaction to prepare bromomalonate dipoly(glycidyl nitrate), and reacting with fullerene to prepare the fullerene poly(glycidyl nitrate). According to the present invention, the fullerene derivative can be used in the solid rocket propellant as a novel energetic combustion catalyst; and experiment results prove that the product yield can be 82%, and the platform combustion rate can be increased by 65% while the pressure index is reduced to 0.21 when the product of the present invention is applied in the solid propellant as the novel combustion catalyst. The formula I is defined in the instruction, wherein n is 2-20.

Description

technical field

[0001] The invention relates to an energetic combustion catalyst and its preparation method and application, in particular to a fullerene polyglycidyl ether nitrate and its preparation method and application. Background technique

[0002] Solid propellant is the energetic material used for launch and propulsion of various land, sea and air missiles and rockets, and plays an important role in the development of missile and aerospace technology. one of the core. According to the requirement of stable operation of the solid engine, it is generally desired that the propellant has a combustion performance with a wide adjustable range of combustion rate and a low pressure index, and this combustion performance is mainly achieved by adding a combustion catalyst. It can be seen that the combustion catalyst is one of the indispensable components to adjust the combustion performance of solid propellants, and is a very critical functional material in the formulation of...

Examples

Embodiment 1

[0035] Embodiment 1: Preparation of fullerene polyglycidyl ether nitrate 3

[0036] (1) 5.54g of monomethyl polyglycidyl ether nitrate, 0.65mL of acid-binding agent triethylamine and 45mL of methylene chloride were put into the reactor, and malonyl chloride (0.59g) was mixed with 50mL of dichloromethane at 0°C. Diluted methyl chloride was slowly added to the solution and reacted at room temperature for 11 h. The reaction solution was washed with water to a pH of about 7.0, dried and then evaporated to remove the solvent to obtain 4.5 g of malonate dimonomethyl polyglycidyl ether nitrate 1 .

[0037] (2) Add 4.5g of the above-mentioned dimethyl malonate dimethyl polyglycidyl ether nitrate 1 and 100mL of methylene chloride in the reaction flask, and drop 1.5g of bromine into the reaction solution dropwise at room temperature until the reaction solution No fading, and then continue to stir the reaction for 6h. After the reaction was completed, it was washed three times with sat...

Embodiment 2

[0044] Embodiment 2: Preparation of fullerene polyglycidyl ether nitrate 3

[0045] (1) Put 2.26g of monomethyl polyglycidyl ether nitrate, 0.56mL of acid-binding agent pyridine and 20mL of dichloromethane into the reactor, add malonyl chloride (0.59g) with 50mL of dichloromethane After dilution, it was slowly dropped into the solution and reacted at room temperature for 11 hours. The reaction solution was washed with water to a pH of about 7.0, dried and then evaporated to remove the solvent to obtain 2.3 g of malonate dimonomethyl polyglycidyl ether nitrate.

[0046] (2) Add 2.3g of the above-mentioned dimethyl polyglycidyl malonate nitrate 1 and 50mL of dichloromethane into the reaction flask, and add 2.0g of N-bromosuccinimide to the reaction solution at room temperature , and then stirred at 60°C for 4h. After the reaction, wash with saturated sodium bromide solution and distilled water three times in sequence, dry with anhydrous sodium sulfate, filter, and distill the ...

Embodiment 3

[0053] Embodiment 3: Preparation of fullerene polyglycidyl ether nitrate 3

[0054] (1) Under nitrogen or argon atmosphere, put 2.27g monomethyl polyglycidyl ether nitrate, 0.60mL acid-binding agent N, N-dimethylformamide and 25mL methylene chloride into the reactor, 40 Dilute malonyl chloride (0.59g) with 50mL of dichloromethane at °C and slowly drop into the solution, and react at room temperature for 6h. The reaction solution was washed with water to a pH of about 7.0, dried and then evaporated to remove the solvent to obtain 2.5 g of malonate dimonomethyl polyglycidyl ether nitrate 1 .

[0055] (2) Add 2.5g of the above-mentioned dimethyl malonate dimethyl polyglycidyl ether nitrate 1 and 50mL of methylene chloride in the reaction flask, and drop 1.7g of bromine into the reaction solution dropwise at room temperature until the reaction solution No fading, and then continue to stir the reaction for 6h. After the reaction was completed, it was washed three times with satur...

technical field

[0001] The invention relates to an energetic combustion catalyst and its preparation method and application, in particular to a fullerene polyglycidyl ether nitrate and its preparation method and application. Background technique

[0002] Solid propellant is the energetic material used for launch and propulsion of various land, sea and air missiles and rockets, and plays an important role in the development of missile and aerospace technology. one of the core. According to the requirement of stable operation of the solid engine, it is generally desired that the propellant has a combustion performance with a wide adjustable range of combustion rate and a low pressure index, and this combustion performance is mainly achieved by adding a combustion catalyst. It can be seen that the combustion catalyst is one of the indispensable components to adjust the combustion performance of solid propellants, and is a very critical functional material in the formulation of...

Examples

Embodiment 1

[0035] Embodiment 1: Preparation of fullerene polyglycidyl ether nitrate 3

[0036] (1) 5.54g of monomethyl polyglycidyl ether nitrate, 0.65mL of acid-binding agent triethylamine and 45mL of methylene chloride were put into the reactor, and malonyl chloride (0.59g) was mixed with 50mL of dichloromethane at 0°C. Diluted methyl chloride was slowly added to the solution and reacted at room temperature for 11 h. The reaction solution was washed with water to a pH of about 7.0, dried and then evaporated to remove the solvent to obtain 4.5 g of malonate dimonomethyl polyglycidyl ether nitrate 1 .

[0037] (2) Add 4.5g of the above-mentioned dimethyl malonate dimethyl polyglycidyl ether nitrate 1 and 100mL of methylene chloride in the reaction flask, and drop 1.5g of bromine into the reaction solution dropwise at room temperature until the reaction solution No fading, and then continue to stir the reaction for 6h. After the reaction was completed, it was washed three times with sat...

Embodiment 2

[0044] Embodiment 2: Preparation of fullerene polyglycidyl ether nitrate 3

[0045] (1) Put 2.26g of monomethyl polyglycidyl ether nitrate, 0.56mL of acid-binding agent pyridine and 20mL of dichloromethane into the reactor, add malonyl chloride (0.59g) with 50mL of dichloromethane After dilution, it was slowly dropped into the solution and reacted at room temperature for 11 hours. The reaction solution was washed with water to a pH of about 7.0, dried and then evaporated to remove the solvent to obtain 2.3 g of malonate dimonomethyl polyglycidyl ether nitrate.

[0046] (2) Add 2.3g of the above-mentioned dimethyl polyglycidyl malonate nitrate 1 and 50mL of dichloromethane into the reaction flask, and add 2.0g of N-bromosuccinimide to the reaction solution at room temperature , and then stirred at 60°C for 4h. After the reaction, wash with saturated sodium bromide solution and distilled water three times in sequence, dry with anhydrous sodium sulfate, filter, and distill the ...

Embodiment 3

[0053] Embodiment 3: Preparation of fullerene polyglycidyl ether nitrate 3

[0054] (1) Under nitrogen or argon atmosphere, put 2.27g monomethyl polyglycidyl ether nitrate, 0.60mL acid-binding agent N, N-dimethylformamide and 25mL methylene chloride into the reactor, 40 Dilute malonyl chloride (0.59g) with 50mL of dichloromethane at °C and slowly drop into the solution, and react at room temperature for 6h. The reaction solution was washed with water to a pH of about 7.0, dried and then evaporated to remove the solvent to obtain 2.5 g of malonate dimonomethyl polyglycidyl ether nitrate 1 .

[0055] (2) Add 2.5g of the above-mentioned dimethyl malonate dimethyl polyglycidyl ether nitrate 1 and 50mL of methylene chloride in the reaction flask, and drop 1.7g of bromine into the reaction solution dropwise at room temperature until the reaction solution No fading, and then continue to stir the reaction for 6h. After the reaction was completed, it was washed three times with satur...

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