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Synthesizing method of 2-nitropropane

A technology for nitropropane and a synthesis method, which is applied in the field of preparation of substituted saturated hydrocarbons, can solve the problems of excessive acetone oxime yield, difficulty in balancing the overall production load, and the like, and achieves the effects of simple post-processing, convenient operation, and mild reaction conditions.

Active Publication Date: 2017-07-28
宁波四明化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is simple, the conditions are mild, the operation is convenient, and the cost of raw materials is low. However, if the market demand for 2-nitropropane is large, the production of acetone oxime is too large and it is difficult to balance the overall production load.

Method used

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  • Synthesizing method of 2-nitropropane
  • Synthesizing method of 2-nitropropane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 6 g (0.1 mol) of acetamide, 58 g (1 moL) of acetone, and 150 g of water into the reaction vessel, and set the temperature of the water bath to 35°C. First slowly pass in about 20-25g of ammonia gas until the temperature in the reaction vessel no longer changes and there is a slight positive pressure in the vessel, raise the temperature and keep the temperature at 40±2°C, add 136g (1.1moL) of 27.5% hydrogen peroxide evenly within 2 hours, drop During the addition, 10 g of ammonia gas was passed into the container 4 times. After the hydrogen peroxide drops, keep warm for 1 hour, and take a sample to detect that the GC content of acetone is <1%, otherwise a small amount of hydrogen peroxide needs to be added.

[0028] Raise the temperature to 75±2°C in the reaction vessel, add 124g (1.0moL) of 27.5% hydrogen peroxide dropwise evenly within 2h, keep it warm for 1h after dropping, drop the temperature to 30-40°C, and add about 15-20g of 31% hydrochloric acid dropwise to ...

Embodiment 2

[0032] The catalyst in the embodiment 1 is replaced by the ammonium acetate catalyst 6g, and the others are the same as in the embodiment 1. After the hydrogen peroxide is dripped for the first time and the heat preservation is finished, the GC content of acetone is 6% in a sample, and 25 g of hydrogen peroxide needs to be added. 67 g of the final product were obtained.

[0033] As detected by GC, the 2-nitropropane content in the final product was 99.0% (wt%), and the total molar yield of 2-nitropropane in terms of acetone was 76%.

Embodiment 3

[0035] Change the amount of acetamide catalyst in Example 1 to 3g, and the others are the same as in Example 1. After the hydrogen peroxide is dripped for the first time and the heat preservation finishes, the GC content of acetone is sampled at 4%, and 20g of hydrogen peroxide needs to be added. 69 g of the final product were obtained.

[0036] As detected by GC, the 2-nitropropane content in the final product was 99.1% (wt%), and the total molar yield of 2-nitropropane in terms of acetone was 78%.

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Abstract

The invention discloses preparation of substituted saturated hydrocarbon and particularly relates to a synthesizing method of 2-nitropropane. The 2-nitropropane is prepared by oxidizing isohydrazone. The synthesizing method includes the steps of S1, condensing acetone, water and ammonia in the presence of a catalyst to generate ketimine, wherein the mass ratio of the acetone to the water is 1:(1-5), and the use amount of the catalyst is 5-11% of the use amount of the acetone; S2, oxidizing the ketimine obtained in the step S1 to form the isohydrazone, wherein reaction system temperature is 30-60 DEG C and heat-preservation reaction time is 0.5-3 hours; S3, oxidizing the isohydrazone obtained in the step S2 to form the 2-nitropropane, wherein reaction system temperature is 50-80 DEG C and heat-preservation reaction time is 0.5-3 hours; rectifying obtained primary reaction liquid to obtain qualified 2-nitropropane products. The synthesizing method has the advantages that the acetone, the ammonia and the water are used as the initial raw materials, and the method is mild in catalytic oxidizing reaction condition, simple in process, convenient to operate, suitable for large-batch 2-nitropropane production, simple in post-processing and high in product purity and does not coproduce acetone oxime or acetone azine.

Description

technical field [0001] The invention relates to a preparation of substituted saturated hydrocarbons, in particular to a synthesis method of 2-nitropropane. Background technique [0002] 2-Nitropropane is an important solvent and pharmaceutical intermediate, and is often used in the synthesis of chloronitroalkane pesticides. The 2-amino-2-methyl-1-propanol obtained by its reduction is a very important surfactant group. [0003] Chinese patent application CN201610208003.3 discloses a method of using acetone, ammonia, hydrogen peroxide, and reaction solvent to synthesize 2-nitropropane and acetone oxime under the action of a titanium-silicon molecular sieve catalyst. The high-purity 2-nitropropane without other nitroalkanes can be obtained through treatment, and at the same time, 30-50% of acetone oxime can be co-produced. The process is simple, the conditions are mild, the operation is convenient, and the cost of raw materials is low. However, if the market demand for 2-nitro...

Claims

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Application Information

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IPC IPC(8): C07C201/06C07C201/16C07C205/02C07D273/01C07C249/02C07C251/08
CPCC07C201/06C07C201/16C07C249/02C07D273/01C07C205/02C07C251/08
Inventor 段云凤罗署柳圣镜李亚东
Owner 宁波四明化工有限公司
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