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Method for synthesizing nitroalkane at low temperature

A technology for nitroalkane and nitrohexane, which is applied in the field of chemical engineering, can solve the problems of high reaction temperature, high pressure, alkane fracture, etc., and achieves the effects of cheap and easy-to-obtain reaction raw materials and low reaction temperature.

Pending Publication Date: 2022-06-28
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] There are still many deficiencies in the above-mentioned preparation method of nitroalkane, such as relatively high requirements for reaction temperature, and relatively high requirements for pressure, but under high temperature and high pressure, the C-C bond of alkane is prone to breakage, so in the reaction product More by-products will appear in the above-mentioned patents, and at the same time, aldehydes and ketones are used as substrates for nitration in the above-mentioned patents.

Method used

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  • Method for synthesizing nitroalkane at low temperature
  • Method for synthesizing nitroalkane at low temperature
  • Method for synthesizing nitroalkane at low temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Accurately pipette 4.31g of n-hexane, 1.293g of TBP and 8.33mL of 2mol L into the Teflon liner -1 HNO 3 , then put the magnet into the PTFE liner and transfer the liner to the kettle sleeve for fixing and sealing, and finally put the kettle sleeve into the heating base, connect the thermocouple and pressure sensor, and set the reaction The temperature is 100°C, and the reaction time is 6h. After the reaction, the sample was taken out, and the sample was washed with alkali with sodium bicarbonate solution, repeated three times, and finally the sample was dried with anhydrous sodium sulfate. The product was then analyzed by GC-MS. The yields of the three nitro compounds were 5.9% for 1-nitrohexane, 33.1% for 2-nitrohexane and 26.3% for 3-nitrohexane.

Embodiment 2

[0039] Process and used reactor are the same as embodiment 1, and difference is that the substance concentration of nitric acid is 10mol / L, and the productive rate of three kinds of nitro compounds is respectively 1-nitrohexane 10.3%, 2-nitrohexane 39.4%, 3-nitrohexane 33.2%.

Embodiment 3

[0041] The process and the reactor used are the same as in Example 1, except that the reaction temperature is 130°C, and the yields of the three nitro compounds are respectively 9.9% for 1-nitrohexane, 37.9% for 2-nitrohexane, and 37.9% for 3-nitrohexane. Nitrohexane 30.6%.

[0042] By embodiment 1 and embodiment 2, illustrate that the nitric acid concentration is higher, and the productive rate of nitrohexane is higher.

[0043] Through embodiment 1 and embodiment 3, illustrate that reaction temperature is higher, and the productive rate of nitrohexane is higher.

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Abstract

The invention provides a method for synthesizing nitroalkane at low temperature, which is carried out in a miniature reaction kettle by taking normal hexane or cyclohexane as a raw material, tributyl phosphate as a solvent and nitric acid as a nitrating agent. By controlling the reaction temperature to be 100-130 DEG C, the concentration of nitric acid to be 2-10 mol / L and the reaction time to be 4-12 h, three nitration products can be obtained from n-hexane, and the yields of 1-nitrohexane, 2-nitrohexane and 3-nitrohexane are 5.9-9.9%, 33.1-37.9% and 26.3-30.6% respectively; the nitration product of cyclohexane is nitrocyclohexane, and the yield of the nitration product is 25.5-40.1%. The preparation method provided by the invention has two advantages: (1) the reaction can be carried out at a lower temperature and a lower nitric acid concentration; (2) the yield of nitroalkane can be adjusted within a certain range; and (3) few by-products are generated in the reaction.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, and mainly relates to a method for obtaining corresponding nitroalkanes at low temperature in a miniature reactor by using short-chain alkanes as raw materials, nitric acid as a nitrating agent, and tributyl phosphate as a solvent. Background technique [0002] Nitroalkane has a wide range of uses. At present, more than 2,000 kinds of its derivatives have been produced, and their uses involve the fields of medicine, pesticides and explosives. [0003] (1) Used as a solvent [0004] Nitromethane is often used as a solvent for various resins, cellulose and polyvinyl chloride due to its low volatility, low toxicity and high boiling point. And because nitromethane has poor solubility to various alkanes, nitromethane can also be used as an extractant for separating naphthalene from gasoline. [0005] (2) Used as fuel and fuel additive [0006] The main component of rocket fuel in the m...

Claims

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Application Information

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IPC IPC(8): C07C205/02C07C205/05C07C201/08
CPCC07C201/08C07C205/02C07C205/05
Inventor 唐双凌王墨
Owner NANJING UNIV OF SCI & TECH
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