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A method for resource utilization of residual nitric acid in the nitration solution of H acid

A technology of nitrification and resource utilization, applied in the preparation of sulfonic acid, organic chemistry, etc., can solve the problems of hidden safety and environmental protection, difficult equipment selection, and high energy consumption.

Active Publication Date: 2017-12-29
JIANGSU YANGNONG CHEM GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this process will produce a large amount of nitrogen oxides and toxic substances, which has great safety and environmental protection risks, and requires long-term high-temperature heat treatment, high energy consumption, and difficult equipment selection. The traditional process of denitrification is achieved by using high-temperature pyrolysis of nitric acid. There are significant issues that need to be resolved

Method used

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  • A method for resource utilization of residual nitric acid in the nitration solution of H acid
  • A method for resource utilization of residual nitric acid in the nitration solution of H acid
  • A method for resource utilization of residual nitric acid in the nitration solution of H acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 47.21g of toluene into a 250mL four-neck flask, stir well, and raise the temperature to 40°C. 123.37g of nitrification solution before denitrification, DVS value of 6.10, and nitric acid content of 2.62%, was added dropwise to a four-neck flask, reacted at 40°C for 1 hour, and then left to separate layers. The obtained water layer was 120.26g, with a nitric acid content of 65ppm. The oil layer is 43.32g, the yield of o-nitrotoluene is 63.38%, and the yield of p-nitrotoluene is 36.62%.

Embodiment 2-4

[0027] On the basis of Example 1, 57.76 g of chlorobenzene was used instead of toluene as the solvent, and other conditions remained unchanged. The obtained results are shown in Table 1.

[0028] Table 1 Chlorobenzene is used as a solvent, and the influence of different reaction times on denitrification

[0029]

Embodiment 5

[0031] Add 40.08g of benzene into a 250mL four-necked flask, stir well, and raise the temperature to 40°C. 123.37g of nitrification solution before denitrification, DVS value of 6.10, and nitric acid content of 2.62%, was added dropwise to a four-neck flask, reacted at 40°C for 1 hour, and then left to separate layers. The obtained water layer was 120.32g, with a nitric acid content of 83ppm. The oil layer is 43.07g, and the yield of nitrobenzene is 99.86%.

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Abstract

The invention relates to a recycling method for residual nitric acid in a nitration solution of a reactive dye intermediate H acid, belonging to the technical field of organic chemical industry. Specifically, the method uses refined naphthalene as a raw material, introduces an organic solvent for an in-situ reaction with residual nitric acid in the nitration solution after sulfonation and nitration, and can control the content of nitric acid to be lower than 100 ppm. The recycling method has the characteristics of safe and environment-friendly production environment, low production cost and low equipment investment.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, and relates to a method for resource utilization of residual nitric acid in the nitration solution of reactive dye intermediate H acid, more specifically, relates to a method of using refined naphthalene as a raw material, after sulfonation and nitration, using Introducing an organic solvent to react in situ with the residual nitric acid in the nitration solution can effectively control the nitric acid content below 100ppm. The present invention is characterized in that the production environment is safe and environment-friendly, the production cost is low and the equipment investment is small. Background technique [0002] H acid (1-amino-8-naphthol-3,6-disulfonic acid monosodium salt) is mainly produced through the following steps: (1) naphthalene sulfonation to obtain 1,3,6-naphthalenesulfonic acid; (2) 1,3,6-naphthalenetrisulfonic acid is nitrated to generate 1-nitro-3,6,8-...

Claims

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Application Information

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IPC IPC(8): C07C309/40C07C303/22
Inventor 王根林丁克鸿王刚胡俊殷恒志陆林华
Owner JIANGSU YANGNONG CHEM GROUP
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