Preparation method of short-chain nitroalkane

A technology for nitroalkane and nitrohexane, which is applied in the field of chemical engineering, can solve the problems of difficult product separation, high reaction pressure and high reaction temperature, and achieves the advantages of cheap and easily available reaction raw materials, low reaction temperature and pressure, and simple operation. Effect

Pending Publication Date: 2022-07-01
NANJING UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0007] The above-mentioned preparation method for the nitration of short-chain alkanes still has many defects, such as (1) the nitration reaction temperature is higher, and higher energy consumption is arranged, and it also causes the fracture of the C-C bond of the alkane in addition, resulting in the need for a separation process; (2) the reaction Oxygen and other oxidants need to be introduced and the reaction pressure is too high, which requires high equipment and poor safety; (3) by using other substrates, such as alcohols, aldehydes and acids as substrates, using catalysts to catalyze, it is difficult to separate products and cost Larger, not conducive to industrial applications

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  • Preparation method of short-chain nitroalkane
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  • Preparation method of short-chain nitroalkane

Examples

Experimental program
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Effect test

Embodiment 1

[0029] In a 50ml micro-reactor, add n-hexane and NO successively 2 , n-hexane and NO 2 The ratio of the amount of substances is 1:1. The reaction temperature was set to 100°C and the reaction time was 4h. After the reaction, the reactor was cooled to room temperature, and then the reactor was safely opened to take out the reaction solution. A 5% aqueous sodium bicarbonate solution was added to the reaction solution to quench the reaction, and the reaction solution was washed with alkali until neutral, then washed with deionized water for several times, and finally dried with anhydrous sodium sulfate to remove water. Since the product nitrohexane is volatile, for the calculation of the yield, we directly take part of the reaction solution after simple treatment for gas chromatography and GC-MS detection and analysis. Under the reaction conditions, the conversion rate of n-hexane was 29.6%, and the selectivity of each product: 1-nitrohexane was 1.2%, 2-nitrohexane was 58.0%, ...

Embodiment 2

[0031] The process and the reactor used are the same as in Example 1, except that the reaction temperature is 120 ° C, and the conversion rate of n-hexane is recorded as 64.3% under the reaction conditions, and the selectivity of each product: the selection of 1-nitrohexane The selectivity was 1.4%, the selectivity of 2-nitrohexane was 57.6%, and the selectivity of 3-nitrohexane was 41.0%.

Embodiment 3

[0033] Process and used reactor are the same as in Example 1, except that n-hexane and NO 2 The ratio of the amount of the substances is 1:2, the conversion rate of n-hexane is 85.9% under this reaction condition, and the selectivity of each product: the selectivity of 1-nitrohexane is 2.0%, the selectivity of 2-nitrohexane is 2.0%, and the The selectivity of nitrohexane was 54.3%, and the selectivity of 3-nitrohexane was 43.7%.

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Abstract

The invention provides a preparation method of short-chain nitroalkane, which is carried out in a miniature reaction kettle by taking normal hexane as a raw material and NO2 as a nitration reagent. Three target products are obtained by controlling the reaction temperature between 100 DEG C and 140 DEG C, the molar ratio of n-hexane to NO2 to be 1: (0.5-2.5) and the reaction time to be 0.5-8 hours, and the selectivity of 1-nitrohexane is 1-3%, the selectivity of 2-nitrohexane is 52-59%, and the selectivity of 3-nitrohexane is 40-47%. The preparation method of the short-chain nitroalkane provided by the invention has the following three advantages: (1) the nitration reaction temperature is low, and no other by-products are generated; (2) no waste acid or waste water is generated in the reaction process, and good environmental friendliness and atom economy are achieved; and (3) the conversion rate and the yield of reactants can be adjusted within a certain range.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, and mainly relates to a kind of short-chain alkane and NO 2 A method for obtaining specific selective nitroalkanes by safe nitration in a micro-reactor. Background technique [0002] Aliphatic nitroalkanes are widely used in national defense, pesticides, pigments, medicine and other fields. (1) The main component of nitromethane-based liquid explosives is nitroalkane, which has a large detonation diameter and is usually used for oil and gas reservoir exploitation; trimethylolnitromethane is nitrified to obtain methyl trinitrate nitromethane, which is It is a kind of high explosive, and its explosive effect is equivalent to that of tetranitropentaerythritol; under certain detonation conditions, nitroalkane can form strong detonation like solid explosives. Large impulse; (2) Nitroalkane can be used as a solvent for vinyl resin, various cellulose, various resins, polyvinyl chloride an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/08C07C205/02
CPCC07C201/08C07C205/02
Inventor 唐双凌李星彦彭新华
Owner NANJING UNIV OF SCI & TECH
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