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Preparation method of 2-chloro-2-nitropropane

A technology of nitropropane and acetone oxime, which is applied in the field of preparation of 2-chloro-2-nitropropane, can solve the problem of low reaction yield and achieve the effect of reducing the cost of raw materials

Pending Publication Date: 2022-06-17
河北旭阳能源有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs two-step reaction, carries out chlorination and oxidation generation 2-chloro-2-nitropropane with chlorine and ozone respectively, and the used chlorination reagent of this method is a kind of hypertoxic gas that has strong pungent smell, and reaction yield rate is lower only 30%

Method used

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  • Preparation method of 2-chloro-2-nitropropane
  • Preparation method of 2-chloro-2-nitropropane
  • Preparation method of 2-chloro-2-nitropropane

Examples

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Effect test

Embodiment 1

[0044] In a 5L three-necked bottle equipped with an electric stirrer, a thermometer and a solid feeding port, 3736.17 g of sodium hypochlorite solution was added at room temperature, and the available chlorine content was 13.0%. Under the conditions of stirring and temperature control at 15°C, 250 g of acetone oxime was added to the three-necked flask in batches, and the addition time was 1.0 h. After the addition was completed, the reaction was continued to stir at room temperature for 0.5 h. After the reaction was completed, the reaction solution was placed in a separatory funnel and left to stand for stratification, and the separated lower layer liquid was 361.29 g of 2-chloro-2-nitropropane product, with a yield of 85.5%. GC detection, purity 99.6%.

Embodiment 2

[0046] In a 5L three-necked flask equipped with an electric stirrer, a thermometer and a solid feeding port, 1810.61 g of sodium hypochlorite solid (content 90%) and 1922.61 g of water were added successively at room temperature. Under the conditions of stirring and temperature control at 15°C, a total of 400 g of acetone oxime was added to the three-necked flask in batches, and the addition time was 1.5 h. After the addition was completed, the reaction was continued to stir at room temperature for 0.5 h. After the reaction was completed, the reaction solution was placed in a separatory funnel to stand for stratification, and the lower layer liquid was separated to obtain 561.16 g of the 2-chloro-2-nitropropane product, with a yield of 83.0%. GC detection, purity 99.5%.

[0047] 2-Chloro-2-nitropropane product yield is mass yield: measure the moisture of the product separated from the separatory funnel by Karl Fischer's moisture measurement method to obtain the purity of the ...

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Abstract

The invention discloses a preparation method of 2-chloro-2-nitropropane, which comprises the following steps: S1, sequentially adding pypocholoride and water into a three-neck flask provided with a thermometer and a solid feeder, then placing the three-neck flask on a constant-temperature heating magnetic stirrer, and stirring at the reaction temperature of 0-50 DEG C; s2, adding the raw material acetoxime into the three-neck flask in batches for reaction; s3, after the reaction is completed, cooling a reaction solution to room temperature, standing and layering in a separating funnel, and separating out a lower-layer solution 2-chloro-2-nitropropane; and S4, the yield of the product 2-chloro-2-nitropropane is 83.0%-85.5%, and the purity detected by GC (Gas Chromatography) is 99.5%-99.6%. The raw material cost is greatly reduced; the method is a synthesis process, and solvent recovery waste and environment pollution caused by use of a large amount of solvent are avoided; the product can be obtained only by standing and layering.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method of 2-chloro-2-nitropropane. Background technique [0002] 2-Chloro-2-nitropropane, also known as 2-nitro-2-chloropropane, is an organic synthesis reagent that can be used to prepare DMNB, a chemical marker for explosives. It is used as a pesticide in agriculture and as a solvent for hydrocarbons in the chemical industry. In recent years, due to the increase in the demand for 2-chloro-2-nitropropane-related manufacturing products, the market demand for 2-chloro-2-nitropropane has expanded, and its industrialization has good market prospects and significant economic benefits. [0003] The synthesis of 2-chloro-2-nitropropane by the chlorination method of 2-nitropropane is a widely used method, and the chlorination reagents are generally chlorine, NCS, carbon tetrachloride, oxalyl chloride and the like. Solvents are generally water, methanol, tetrahydrofuran,...

Claims

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Application Information

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IPC IPC(8): C07C201/06C07C205/08
CPCC07C201/06C07C205/08
Inventor 何海娜王立平王耀红李韶辉王英其娄瑞娟曹亚林路广乾
Owner 河北旭阳能源有限公司
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