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A kind of continuous oxidation method for preparing hexanoic acid by oxidizing sec-octanol with nitric acid

A technology of nitric acid oxidation and sec-octanol, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of low oxidation efficiency, time-consuming and energy-consuming, and potential safety hazards, so as to improve production Efficiency, reduce warm-up response time, save power and energy

Inactive Publication Date: 2015-08-19
河北科正化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to provide a continuous oxidation method for preparing hexanoic acid by oxidizing sec-octanol with nitric acid, so as to solve the problems of time-consuming and energy-consuming, low oxidation efficiency, and large safety hazards in the existing process.

Method used

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  • A kind of continuous oxidation method for preparing hexanoic acid by oxidizing sec-octanol with nitric acid

Examples

Experimental program
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Embodiment 1

[0026] Such as figure 1 As shown, in a mixing tower body 1 with a diameter of 1000 mm, a heating device 2 and a material circulation pump 3 are installed at the bottom of the tower, and 10 bubble-cap plates 4 are installed in the lower half of the tower (from top to bottom are the 1st to 10th plates), The upper half of the tower is equipped with upper, middle and lower packing layers respectively, corresponding to packing layer 5-a, packing layer 5-b and packing layer 5-c respectively, packing layer 5-a, packing layer 5-b and The upper part of the packing layer 5-c is respectively provided with a liquid spray pipe 6-a, a spray pipe 6-b and a spray pipe 6-c, and the lower part of the packing layer 5-a and the packing layer 5-b is respectively provided with a liquid collecting plate 7 -a, the liquid collecting plate 7-b, the uppermost part of the mixing tower is provided with an exhaust gas outlet 8, which is connected with the exhaust gas recovery system, and the lowermost part...

Embodiment 2

[0028] In this embodiment, a packed tower is used, that is, the 10-plate blister plate in the lower half of the tower in Example 1 is converted into 14 packing layers, and the entire packed tower is 17 packing layers (from top to bottom 1-17). The specific process is as follows : Use a pump to add the 2-octanol mixed with the catalyst to the third section of the packing layer through the spray pipe, directly flow into the fourth and fifth sections of the packing layer until the bottom of the tower, stop feeding when the material circulation pump can circulate, and turn on the heating device to When the temperature in the tower rises to 90°C, use a pump to add 40% nitric acid into the second packing layer through the spray pipe, continue heating and material circulation, and when the temperature is maintained at 100°C and yellow smoke comes out from the top of the tower, the reaction proceeds normally. , stop heating; at the same time, add 2-octanol mixed with catalyst at a flow...

Embodiment 3

[0030]This embodiment adopts a plate tower, that is, the three-stage packing layer in the upper half of the tower in Example 1 is converted into an 8-plate blister plate, and three spray pipes are respectively arranged on the top of the 1st, 5th, and 7th plates of the blister plate. The liquid collecting plates are respectively arranged at the lower part of the 4th and 6th plates of the blister plate, and the specific process is as follows: the secondary octanol mixed with the catalyst is added to the 7th plate of the blister plate through the spray pipe through the pump, and directly flows into the blister plate From the 8th and 9th plates to the bottom of the tower, stop feeding when the material circulation pump can circulate, turn on the heating device until the temperature in the tower rises to 110°C, use a pump to add 40% nitric acid to the fifth plate of the blister plate through the spray pipe, Continue heating and material circulation, and stop heating when the tempera...

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Abstract

The invention discloses a continuous oxidation method for preparing hexanoic acid by using nitric acid oxidation octanol, belonging to the technical field of hexanoic acid production. The method is an improvement of a process with the defects of material accumulation in original reaction and difficultly determined addition amount and time of nitric acid, and gas generated through the reaction is more easily escaped from a liquid level through reducing the thickness of a reaction liquid and increasing the gas escape area by using a material layered reaction method, thus material overflow and explosion accidents are fundamentally stopped. By using the method, the concentrations of materials at different layers or the number of layers of the materials can be adjusted, so that the reaction selectivity can be controlled. In addition, a method for recollecting steam generated by reaction to preheat the materials so as to recycle the heat energy is adopted, so that not only can the electrical energy be saved, but also the preheating reaction time is shortened. In addition, a continuous feeding oxidation method is adopted, so that the production efficiency of the oxidation process for producing hexanoic acid by using nitric acid oxidation octanol is fundamentally increased.

Description

technical field [0001] The invention relates to a continuous oxidation method for preparing caproic acid by oxidizing sec-octanol with nitric acid, and belongs to the technical field of caproic acid production. Background technique [0002] As a basic low-carbon organic acid, caproic acid is widely used in industries such as pharmaceuticals, organic synthesis, and fragrances, especially in the fragrance industry. Ethyl caproate and allyl caproate synthesized from it are both bulk fragrance products. The hexanoic acid manufacturers in our country all adopt the method of nitric acid to oxidize 2-octanol to produce hexanoic acid. The process flow is roughly as follows: Preheat 2-octanol and catalyst to a certain temperature in the kettle reactor, add nitric acid dropwise for oxidation, and carry out after the reaction is completed. Wash with water, and then decompress and fractionate the oil layer to obtain hexanoic acid. Briefly the process includes three sections, namely oxi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/126C07C51/27
CPCC07C51/27C07C53/126
Inventor 谷长安谷利敏
Owner 河北科正化工有限公司
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