Method for reclaiming nitric acid from nitrified waste acid

A technology for nitrating waste acid and nitric acid, applied in the direction of nitric acid, nitrogen oxides/oxyacids, etc., can solve problems such as equipment corrosion, and achieve the effect of reducing corrosion

Inactive Publication Date: 2012-03-28
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs to remove the nitric acid in the nitrification waste acid by bubbling hot air. During the nitric acid removal process, nitrogen oxides and water are generated, which is easy to cause corrosion to the equipment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 300 grams of nitration waste acid, add 47.3 grams of 1,2,3-trichlorobenzene (the same amount as the nitration raw material), start stirring, raise the temperature to 50 ° C, maintain the reaction, and take a sample once every 30 minutes to reach the organic component No change, organic content: 1,2,3-trichlorobenzene 74.56%, 1,2,3-trichlorobenzene-4-nitrobenzene 24.05%. After the above reaction solution was left to stand and separated, the weight of the organic phase increased by 3.8 grams, and the organic phase was added to the mixed acid (containing 290 grams of 98% sulfuric acid and 194 grams of 65% nitric acid), and the temperature was raised to 90 ° C, and the reaction was maintained for 3 hours. After standing still, the organic phase components contained 95.86% of 1,2,3-trichlorobenzene-4,6-dinitrobenzene and 0.11% of 1,2,3-trichlorobenzene-4-nitrobenzene.

[0022] Explanation: The source of nitrification waste acid is the following comparative example 1, in...

Embodiment 2

[0024] Take 300 grams of nitration waste acid, add 23.6 grams of 1,2,3-trichlorobenzene (50% of the amount of nitration raw material), start stirring, raise the temperature to 50 ° C, maintain the reaction, and take a sample once every 30 minutes to reach the organic matter. The components do not change anymore, the organic content: 1,2,3-trichlorobenzene 54.67%, 1,2,3-trichlorobenzene-4-nitrobenzene 42.55%. After the above reaction solution was left to stand and separated, the weight of the organic phase increased by 3.8 grams, and the organic phase and 23.7 grams of 1,2,3-trichlorobenzene were added to the mixed acid (290 grams of 98% sulfuric acid, 194 grams of 65% nitric acid), Raise the temperature to 90°C, maintain the reaction for 3 hours, and let it stand still. The organic phase component content is 97% of 1,2,3-trichlorobenzene-4,6-dinitrobenzene, - Nitrobenzene 0.05%.

Embodiment 3

[0026] Take 300 grams of nitration waste acid, add 16.5 grams of 1,2,3-trichlorobenzene (35% of the amount of nitration raw material), start stirring, raise the temperature to 50 ° C, maintain the reaction, and take a sample once every 30 minutes to reach the organic matter. The components do not change anymore, the organic content: 1,2,3-trichlorobenzene 32.38%, 1,2,3-trichlorobenzene-4-nitrobenzene 62.59%. After the above reaction solution was left to stand and separated, the weight of the organic phase increased by 3.4 grams, and the organic phase and 30.8 grams of 1,2,3-trichlorobenzene were added to the mixed acid (containing 290 grams of 98% sulfuric acid and 194 grams of 65% nitric acid) , heat up to 90°C, maintain the reaction for 3 hours, and let it stand still. The organic phase component content is 95.87% of 1,2,3-trichlorobenzene-4,6-dinitrobenzene, 1,2,3-trichlorobenzene -4-Nitrobenzene 0.35%.

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PUM

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Abstract

The invention belongs to the technical field of organic chemical nitrification reactions, and relates to a method for reclaiming nitric acid from nitrified waste acid. The method comprises the following steps of: adding a nitrified raw material into the nitrified waste acid, starting to stir, heating to a reaction temperature, and maintaining the reaction until the nitric acid in the nitrified waste acid is completely transformed; standing, and separating organic matters and the waste acid; and adding the organic matters into mixed acid for secondary nitrification, raising the temperature and maintaining the temperature until the reaction is completely performed. The method is used to remove oxynitride in the waste acid by recycling the nitric acid in the nitrified waste acid, so that corrosion of equipment is reduced; and the consumption of the nitric acid in the nitrifying process is reduced, and the production cost is reduced. According to the invention, the dose of the nitric acid in the nitrification reaction is reduced by sufficiently utilizing the nitric acid component in the nitrified waste acid; and the waste acid is concentrated after the nitric acid in the waste acid is reclaimed, and the corrosion of the oxynitride generated in the waste acid reclaiming process to reclaim equipment is reduced.

Description

technical field [0001] The invention belongs to the technical field of organic chemical nitration reaction, and relates to a method for recovering nitric acid from nitration waste acid. Background technique [0002] Nitrification reaction is a commonly used organic reaction, which is a reaction in which organic materials are heated up in a mixed acid prepared by sulfuric acid and nitric acid to prepare organic matter. In order to improve the conversion rate of organic matter in the nitration reaction, the molar number of nitric acid in the mixed acid is usually higher than the theoretical value of nitric acid required for complete nitration of organic matter. After the nitration reaction is completed, the organic phase is separated, and excess nitric acid remains in the sulfuric acid to form nitration waste acid. There are generally two ways to treat waste nitrification acid: one is to use the waste nitrification acid for the production of ammonium sulfate; the other is to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/46
Inventor 王培兰邹宁芬何育苗
Owner CHINA PETROLEUM & CHEM CORP
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