Preparing method of low-carbon nitroparaffins

A technology for nitroalkane and nitropropane, which is applied in the field of safe gas-phase nitration to obtain nitroalkane with specific selectivity, can solve the problem that the specific selectivity of nitrification products cannot be completely solved.

Inactive Publication Date: 2014-08-27
嘉兴润博化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] What the present invention aims to solve is the defect that the specific selectivity of the nitration product cannot be completely solved in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The invention adopts a multi-channel reactor to carry out the nitrification reaction. The molar ratio of propane and nitric acid is 6:1, and the operating pressure is 0.1Mpa. Propane enters the reaction channel port through the flowmeter, and nitric acid is pumped into the reaction channel port through the metering pump. The materials are fully mixed in the mixing chamber and then enter the reactor. The reaction temperature is 340 °C, residence time 0.8s, continuous reaction for 1h, the product flows out from the outlet after being condensed in the collection chamber, the obtained product is separated, the upper layer is an organic phase, and the lower layer is an aqueous phase. The upper layer was analyzed by gas chromatography, and the selectivities of the four nitro compounds were 4.4% for nitromethane, 11% for nitroethane, 41.6% for 1-nitropropane, and 44% for 2-nitropropane.

Embodiment 2

[0019] The process and the reactor used are the same as in Example 1, except that the molar ratio of propane to nitric acid is 2:1, the operating pressure is 0.5Mpa, and the residence time is 1.4s. The selectivities of the four nitro compounds were 6.7% for nitromethane, 12.2% for nitroethane, 42% for 1-nitropropane, and 39.1% for 2-nitropropane.

Embodiment 3

[0021] The process and the reactor used are the same as in Example 1, except that the reaction temperature is 435°C. The selectivities of the four nitro compounds were 7% for nitromethane, 13% for nitroethane, 45% for 1-nitropropane, and 35% for 2-nitropropane.

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PUM

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Abstract

The invention provides a preparing method of low-carbon nitroparaffins. According to the method, a reaction is carried out in a multi-passage heat insulation reaction vessel by using propane as raw materials and using nitric acid as nitrating agents; four kinds of target products are obtained through controlling the reaction temperature to be 300 to 450 DEG C, the pressure to be 0 to 1.0 Mpa, the dwell time to be 0.5 to 2s and the mol ratio of the propane to the nitric acid to be (2-6):1; the selectivity of nitromethane is 4 to 7 percent; the selectivity of nitroethane is 9 to 13 percent; the selectivity of 1-nitropropane is 40 to 45 percent; and the selectivity of 2-nitropropane is 35 to 40 percent. The preparing method of the low-carbon nitroparaffins provided by the invention mainly has two major advantages that (1) four kinds of nitroparaffins with specific selectivity can be simultaneously obtained; and (2) the selectivity of nitration products is adjustable in a certain range.

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 obtaining specific and selective nitroalkanes by safe gas-phase nitration in a multi-channel reactor using propane and nitric acid as raw materials. Background technique [0002] The preparation of low-carbon nitroalkanes is mainly based on nitric acid as a nitrating agent, and low-carbon alkanes and alkanes undergo gas phase reactions at high temperatures. The gas-phase nitration method of methane mainly includes the thermal decomposition of nitric acid to form free radicals, and then the gas-phase nitration of methane and free radicals to generate nitromethane and water. Using ethane as raw material, it can directly react with nitric acid under pressure to produce nitromethane and nitroethane at the same time. The propane nitration method is to put propane into the preheater to preheat at 430-450°C, and then enter the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/08C07C205/02
Inventor 倪平李沈巍
Owner 嘉兴润博化工科技有限公司
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