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Method for preparing 2-nitropropane

A technology of nitropropane and acetone, applied in the field of organic compound synthesis, can solve problems such as difficult separation, high temperature and high pressure in the reaction process, serious environmental pollution, etc., and achieve the effect of simple reaction process, mild reaction conditions and high selectivity

Inactive Publication Date: 2016-10-26
定州旭阳科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction process of this method is high temperature and high pressure, difficult to separate, and serious environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The synthetic reaction of a, 2-nitropropane

[0021] Add acetone, water and catalyst TS-1 titanium-silicon molecular sieve into the reactor at a mass ratio of 1:2.0:0.3, heat the above reaction system at a reaction temperature of 70°C, add ammonia water (containing 25wt% ammonia) and hydrogen peroxide (containing super Hydrogen oxide 30 wt %), the molar ratios of ammonia water and hydrogen peroxide to acetone were 2:1, 1.6:1, respectively, the reaction time was 8 hours, and the pressure of the reaction system was normal pressure. The results of gas chromatography detection and analysis showed that the conversion rate of acetone was 99%, the selectivity of 2-nitropropane was 58%, and the selectivity of acetone oxime was 40%.

[0022] b, the purification of 2-nitropropane

[0023] After the above reaction is completed, under normal pressure, rectify the 2-nitropropane reaction solution, the reflux ratio is 2:1, 70°C~90°C is the 2-nitropropane distillate, and the product ...

Embodiment 2

[0025] a. Synthesis reaction of 2-nitropropane (reduce the reaction temperature)

[0026] Add acetone, water and catalyst TS-1 titanium-silicon molecular sieve into the reactor at a mass ratio of 1:2.0:0.3, heat the above reaction system at a reaction temperature of 60°C, add ammonia water (containing 25wt% ammonia) and hydrogen peroxide (containing super Hydrogen oxide 30 wt %), the molar ratios of ammonia water and hydrogen peroxide to acetone were 2:1, 1.6:1, respectively, the reaction time was 8 hours, and the pressure of the reaction system was normal pressure. The detection and analysis results show that the conversion rate of acetone is 95%, the selectivity of 2-nitropropane is 50%, and the selectivity of acetone oxime is 45%.

[0027] b, the purification of 2-nitropropane

[0028] After the above reaction is finished, rectify the 2-nitropropane reaction solution, separate layers of the distillate, and wash the oil layer with water to obtain 2-nitropropane, the same as...

Embodiment 3

[0030] a. The synthesis reaction of 2-nitropropane (increase the reaction temperature)

[0031] Add acetone, water and catalyst TS-1 titanium-silicon molecular sieve into the reactor at a mass ratio of 1:2.0:0.3, heat the above reaction system at a reaction temperature of 80°C, add ammonia water (containing 25wt% ammonia) and hydrogen peroxide (containing super Hydrogen oxide 30 wt %), the molar ratios of ammonia water and hydrogen peroxide to acetone were 2:1, 1.6:1, respectively, the reaction time was 8 hours, and the pressure of the reaction system was normal pressure. The detection and analysis results showed that the conversion rate of acetone was 99%, the selectivity of 2-nitropropane was 59%, and the selectivity of acetone oxime was 25%.

[0032] b, the purification of 2-nitropropane

[0033] After the above reaction is finished, rectify the 2-nitropropane reaction solution, separate layers of the distillate, and wash the oil layer with water to obtain 2-nitropropane, ...

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PUM

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Abstract

The invention discloses a method for preparing 2-nitropropane, and relates to the technical field of organic compound synthesis. The method comprises the following steps: enabling acetone, ammonia gas or ammonia water, hydrogen peroxide, a solvent and a catalyst to contact, heating till the reaction temperature of 30-100 DEG C, and controlling the reaction pressure to 0.1-0.2MPa to react, thereby obtaining 2-nitropropane, wherein the catalyst is a TS-1 titanium silicalite molecular sieve; the solvent is water; the mole ratio of acetone to ammonia gas or ammonia water is 1:(1-3); the mole ratio of acetone to hydrogen peroxide is 1:(0.5-2); and the mass ratio of acetone to the catalyst is 1:(0.2-0.4). The method disclosed by the invention has the advantages that the conversion rate of acetone is high and the selectivity of 2-nitropropane is good; the method is simple in reaction process, gentle in reaction condition, environment-friendly and easy in industrial production; and development of environment-friendly chemicals is promoted.

Description

technical field [0001] The invention relates to the technical field of organic compound synthesis. Background technique [0002] 2-Nitropropane is used as a special solvent for ethylene and epoxy resin coatings, rocket fuel, gasoline additives, etc., and is also used in organic synthesis. This product has a strong dissolving ability, and is an excellent solvent for various cellulose derivatives, vinyl resins, etc. It is also used as a solvent for wax, fat, dyes, etc., a lubricant for grinding pigments, and a cleaning and mordant agent for cotton fabrics. [0003] Regarding the preparation method of 2-nitropropane, it is mainly propane nitration method now. Inject 75% nitric acid into the propane gas at 430-450°C in the reaction tower, and the molar ratio of propane to nitric acid is 5:1. The resulting product is nitromethane 10%-30%, nitroethane 20%-25%, 1-nitropropane 25%, 2-nitropropane 40%. The product can also be obtained by nitration of propylene. The reaction proce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/06C07C201/16C07C205/02
CPCC07C201/06C07C201/16C07C205/02
Inventor 王英其孟祥杨克明王锋曹亚林周林肖根林王军俏
Owner 定州旭阳科技有限公司
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