Piperazine cation-base ionic liquid containing ammonia and boron groups and preparation method thereof

Abstract

Te invention discloses piperazine cation-base ionic liquid containing ammonia and boron groups and a preparation method thereof. The preparation method comprises the steps of introducing the ammonia and boron groups into piperazine cation-base ionic liquid, and generating replacement reaction by virtue of a piperazine onium-salt borane complex and sodium salt or silver salt of anions, so as to obtain the piperazine cation-base ionic liquid containing the ammonia and boron groups. The product has very high combustion gas discharging amount and has potential application values in the field of natural liquid propellants; and the preparation method is simple, mild and easy to implement.

Description

technical field

[0001] The invention relates to the technical field of liquid propellants, in particular to a piperazine cation-based ionic liquid containing an ammonia boron group and a preparation method thereof Background technique

[0002] In aerospace and national defense military fields (such as strategic and tactical missiles), propellant is one of the core key technologies. Currently, liquid propellants are still the most widely used propellants in the world. Pyrophoric propellant is the most representative type of liquid propellant. Hydrazine and methylated derivatives of hydrazine are the most commonly used propellant fuels in the world. However, hydrazine compounds are highly volatile, highly toxic and highly carcinogenic, which are very harmful to the environment and human health, and their transportation and storage costs are greatly increased due to their flammability and strong volatility. With the continuous development of manned spaceflight technology and ...

Examples

Embodiment 1

[0021] Dissolve 1.78g of sodium dicyanamide (89g / mol) in water, add 4.38g of silver nitrate (219g / mol), and stir magnetically until a large amount of white solid silver dicyanamide appears in the solution. After the solution is suction filtered, the white solid dicyandiamide Amine silver protected from light for later use.

[0022] Add 30ml of methanol, 0.95g of N-methylpiperazine (100.16g / mol), 2.1g of 2-bromoethylamine hydrobromide (204.89g / mol) into a 100ml single-necked bottle, stir magnetically, and react at room temperature for 15 hours. The solution was extracted several times with dichloromethane to give the piperazinium salt as a liquid. Add 25ml of borane tetrahydrofuran solution with a borane concentration of 1.0M, stir magnetically, and heat in an oil bath at 75°C for 10h. After returning to room temperature, the tetrahydrofuran solution was spin-dried to obtain a borane complex of piperazinium salt. Dissolve the obtained piperazinium salt borane complex in 30ml ...

Embodiment 2

[0024] Dissolve 1.78g of sodium dicyanamide (89g / mol) in water, add 4.38g of silver nitrate (219g / mol), and stir magnetically until a large amount of white solid silver dicyanamide appears in the solution. After the solution is suction filtered, the white solid dicyandiamide Amine silver protected from light for later use.

[0025] Add 35ml of methanol, 1.71g of N-ethylpiperazine (114.16g / mol), 2.41g of 3-bromopropylamine hydrobromide (218.92g / mol) in a 100ml single-necked bottle, magnetically stir, and react at room temperature for 18 hours. The solution was extracted several times with dichloromethane to give the piperazinium salt as a liquid. Add 25ml of borane tetrahydrofuran solution with a borane concentration of 1.0M, stir magnetically, and heat in an oil bath at 75°C for 12h. After returning to room temperature, the tetrahydrofuran solution was spin-dried to obtain a borane complex of piperazinium salt. Dissolve the obtained piperazinium salt borane complex in 30ml o...

Embodiment 3

[0027]Under magnetic stirring at 0-5°C, add 3.73 g of potassium hydroxide (dissolved in 25 ml of ethanol) dropwise into 60 ml of ethanol solution of 8.64 g of dinitroaminopropionitrile, stir at 20°C for 30-40min, then cool to 0°C , Filtrated to obtain 5.3g potassium dinitramide (131g / mol). Dissolve potassium dinitramide in water, add 8.96 g of silver nitrate (219 g / mol), stir magnetically until a large amount of white solid silver dinitrate appears in the solution, and filter the solution to avoid light for later use.

[0028] Add 35ml of methanol, 1.71g of N-methylpiperazine (100.16g / mol), 2.41g of 3-bromopropylamine hydrobromide (218.92g / mol) successively in a 100ml single-necked bottle, stir magnetically, and react at room temperature for 15h. The solution was extracted several times with dichloromethane to give the piperazinium salt as a liquid. Add 25ml of borane tetrahydrofuran solution with a borane concentration of 1.0M, stir magnetically, and heat in an oil bath at 7...

technical field

[0001] The invention relates to the technical field of liquid propellants, in particular to a piperazine cation-based ionic liquid containing an ammonia boron group and a preparation method thereof Background technique

[0002] In aerospace and national defense military fields (such as strategic and tactical missiles), propellant is one of the core key technologies. Currently, liquid propellants are still the most widely used propellants in the world. Pyrophoric propellant is the most representative type of liquid propellant. Hydrazine and methylated derivatives of hydrazine are the most commonly used propellant fuels in the world. However, hydrazine compounds are highly volatile, highly toxic and highly carcinogenic, which are very harmful to the environment and human health, and their transportation and storage costs are greatly increased due to their flammability and strong volatility. With the continuous development of manned spaceflight technology and ...

Examples

Embodiment 1

[0021] Dissolve 1.78g of sodium dicyanamide (89g / mol) in water, add 4.38g of silver nitrate (219g / mol), and stir magnetically until a large amount of white solid silver dicyanamide appears in the solution. After the solution is suction filtered, the white solid dicyandiamide Amine silver protected from light for later use.

[0022] Add 30ml of methanol, 0.95g of N-methylpiperazine (100.16g / mol), 2.1g of 2-bromoethylamine hydrobromide (204.89g / mol) into a 100ml single-necked bottle, stir magnetically, and react at room temperature for 15 hours. The solution was extracted several times with dichloromethane to give the piperazinium salt as a liquid. Add 25ml of borane tetrahydrofuran solution with a borane concentration of 1.0M, stir magnetically, and heat in an oil bath at 75°C for 10h. After returning to room temperature, the tetrahydrofuran solution was spin-dried to obtain a borane complex of piperazinium salt. Dissolve the obtained piperazinium salt borane complex in 30ml ...

Embodiment 2

[0024] Dissolve 1.78g of sodium dicyanamide (89g / mol) in water, add 4.38g of silver nitrate (219g / mol), and stir magnetically until a large amount of white solid silver dicyanamide appears in the solution. After the solution is suction filtered, the white solid dicyandiamide Amine silver protected from light for later use.

[0025] Add 35ml of methanol, 1.71g of N-ethylpiperazine (114.16g / mol), 2.41g of 3-bromopropylamine hydrobromide (218.92g / mol) in a 100ml single-necked bottle, magnetically stir, and react at room temperature for 18 hours. The solution was extracted several times with dichloromethane to give the piperazinium salt as a liquid. Add 25ml of borane tetrahydrofuran solution with a borane concentration of 1.0M, stir magnetically, and heat in an oil bath at 75°C for 12h. After returning to room temperature, the tetrahydrofuran solution was spin-dried to obtain a borane complex of piperazinium salt. Dissolve the obtained piperazinium salt borane complex in 30ml o...

Embodiment 3

[0027]Under magnetic stirring at 0-5°C, add 3.73 g of potassium hydroxide (dissolved in 25 ml of ethanol) dropwise into 60 ml of ethanol solution of 8.64 g of dinitroaminopropionitrile, stir at 20°C for 30-40min, then cool to 0°C , Filtrated to obtain 5.3g potassium dinitramide (131g / mol). Dissolve potassium dinitramide in water, add 8.96 g of silver nitrate (219 g / mol), stir magnetically until a large amount of white solid silver dinitrate appears in the solution, and filter the solution to avoid light for later use.

[0028] Add 35ml of methanol, 1.71g of N-methylpiperazine (100.16g / mol), 2.41g of 3-bromopropylamine hydrobromide (218.92g / mol) successively in a 100ml single-necked bottle, stir magnetically, and react at room temperature for 15h. The solution was extracted several times with dichloromethane to give the piperazinium salt as a liquid. Add 25ml of borane tetrahydrofuran solution with a borane concentration of 1.0M, stir magnetically, and heat in an oil bath at 7...

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