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Safe method for preparing nitropropane by vapor-phase nitration

A nitropropane, gas-phase technology, applied in the preparation of nitro compounds, organic chemistry, etc., can solve the problems of low conversion rate and selectivity of low-carbon alkanes and nitrogen oxides, poor safety, and the need to improve the selectivity of nitropropane, etc. To achieve the effect of simple structure, easy operation, safe and continuous process

Inactive Publication Date: 2011-06-01
中国科学院嘉兴绿色化学工程中心 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process cancels the nitric acid recovery system and shortens the nitrification reaction process, but due to the need to introduce air, the reaction system may be on the edge of the explosion limit at any time, the safety is poor, and the conversion rate and selectivity of low-carbon alkanes and nitrogen oxides are low. nitric acid nitration process
[0004] The above published patents fail to completely solve the problem of nitrification safety, and the conversion rate of propane and the selectivity of nitropropane also need to be improved

Method used

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  • Safe method for preparing nitropropane by vapor-phase nitration
  • Safe method for preparing nitropropane by vapor-phase nitration

Examples

Experimental program
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Embodiment 1

[0022] Such as figure 1 Shown, the present invention adopts single channel reactor to carry out nitration and prepare nitropropane. The inner diameter of the reaction pipe is 4 mm, the length is 1000 mm, the aspect ratio is 250:1, and the specific surface area is 0.82. The volume of the reaction pipe 1: the volume of the mixing pipe 2: the volume of the preheating pipe 3 = 1: 0.6: 0.6. The molar ratio of propane and 65wt% nitric acid is 4:1, the operating pressure is 0.1Mpa, propane enters the preheating pipeline 3 through the flowmeter, the preheating temperature is 350°C, the nitric acid is pumped into the tee port 4 through the metering pump, and the mixing temperature is 250°C , The materials are fully mixed in the mixing pipe 2 and then enter the reaction pipe 1, the reaction temperature is 440°C, the residence time is 0.8s, and the reaction is 1h. The product is condensed by the separator and then separated. The upper layer is the organic phase and the lower layer is the...

Embodiment 2

[0024] The process and the reactor used are the same as in Example 1, except that the molar ratio of propane and nitric acid is 2:1, the operating pressure is 0.5Mpa, and the residence time is 1.4s. The conversion rate of propane is 22.3%, and the selectivity of nitropropane is 81.7% %.

Embodiment 3

[0026] The process and the reactor used are the same as in Example 1, except that the mixing temperature is 200°C, the preheating temperature is 300°C, and the reaction temperature is 435°C. The conversion of propane was 20.8%, and the selectivity to nitropropane was 84.4%.

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Abstract

The invention relates to a safe method for preparing nitropropane by vapor-phase nitration, which comprises the following steps: carrying out reaction in a single-channel reactor, wherein after the reaction material propane enters a preheating pipe via a flowmeter and is mixed with pumped nitric acid in a mixing pipe, the mixed materials are sent into a reaction pipe, and the mol ratio of the propane to the nitric acid is controlled at (1-8):1; the mixed materials are subjected to nitration reaction by mass transfer and heat transfer in the reaction pipe, and the products enter a separator; and the reaction products stand in the separator until the reaction products stratify, the organic phase is separated from the water phase, and the organic phase is washed and dried to obtain the product. By using the invention, the propane and the nitric acid can be directly synthesized into various nitroparaffins under the condition of no catalyst, and the process is safe and continuous. The masstransfer and heat transfer are completed in the single channel without additional heat dissipation, thereby reducing the power consumption. The invention has the advantage of simple structure and is easy to operate. The conversion rate of the propane is higher than 20%, and the selectivity of the nitropropane is higher than 80%.

Description

technical field [0001] The invention relates to a technology for preparing nitroalkanes by gas-phase nitration of alkanes, in particular to a method for preparing nitropropane by safe gas-phase nitration in a single-channel reactor using propane and nitric acid as raw materials. Background technique [0002] Nitration of propane is an important reaction in the chemical industry, and its products include nitromethane, nitroethane, 1-nitropropane and 2-nitropropane. As important fine chemicals, nitroalkanes are the key raw materials for many high value-added pharmaceutical intermediates and chemical reagents. Nitropropane is the key raw material for the synthesis of 2-aminoisobutanol, Key raw materials for propanol, N-isopropylhydroxylamine and 4,4-dimethyloxazoline. The development of fine chemical industry is guaranteed by the progress of alkane nitration technology. [0003] Nitration of alkanes is the introduction of nitro groups to organic carbon atoms, which is a stron...

Claims

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Application Information

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IPC IPC(8): C07C205/02C07C201/08
Inventor 倪平李沈巍王甫来
Owner 中国科学院嘉兴绿色化学工程中心
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