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Copper sulfate recovery treatment process in production process of o-methyl formate benzenesulfonamide

A technology of methyl o-formate benzenesulfonamide and production process, applied in the field of waste liquid treatment, can solve problems such as inapplicability, and achieve the effects of convenient operation, improved efficiency and simple process flow

Pending Publication Date: 2022-06-14
河北允升精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention proposes a copper sulfate recycling process in the production process of methyl o-formate benzenesulfonamide, which solves the problem that the existing process for recovering copper sulfate is not suitable for methyl o-formate benzenesulfonamide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] S1, 3000L copper-containing wastewater mother liquor added to sodium hydroxide for neutralization and treatment to adjust the pH to 7.4, press filter to make copper hydroxide;

[0025]S2, the copper hydroxide obtained by S1 is dissolved in water, slowly add concentrated sulfuric acid, the amount of concentrated sulfuric acid is added to the molar ratio of the copper ion content in the mother liquor of the copper-containing wastewater is 1.2:1, and the control drop-added temperature does not exceed 50 °C;

[0026] S3, after the dropwise addition, the copper hydroxide is stirred for 1.5h to completely dissolve, and the mass of the copper hydroxide is 1.5 times that of the concentrated sulfuric acid in step S2, and the control temperature in the process does not exceed 50 °C;

[0027] S4, add activated carbon stirring for 1h, the control temperature in the process does not exceed 50 °C, after the end of the stirring, no cooling treatment, directly filtered;

[0028] S5, filtra...

Embodiment 2

[0032] S1, 3000L copper-containing wastewater mother liquor is added to sodium hydroxide for neutralization and treatment to adjust the pH to 7.2, and the filter is made of copper hydroxide;

[0033] S2, the resulting copper hydroxide obtained by S1 is dissolved in water, slowly add concentrated sulfuric acid, the amount of concentrated sulfuric acid is added to the molar ratio of the copper ion content in the copper-containing wastewater mother liquor is 1.3:1, and the control drop-added temperature does not exceed 50 °C;

[0034] S3, after the drop addition, after the addition of copper hydroxide stirred for 1.5h found not completely dissolved, at this time slowly add concentrated sulfuric acid, until completely dissolved, the control temperature in the process does not exceed 50 ° C, the quality of copper hydroxide is 2 times the concentrated sulfuric acid in the step S2;

[0035] S4, add activated carbon stirring for 2h, the control temperature in the process does not exceed 5...

Embodiment 3

[0040] S1, 3000L copper-containing wastewater mother liquor is added to sodium hydroxide for neutralization and treatment to adjust the pH to 7.31, and press filter to make copper hydroxide;

[0041] S2, the copper hydroxide obtained by S1 is dissolved in water, slowly add concentrated sulfuric acid, the amount of concentrated sulfuric acid is added to the molar ratio of the copper ion content in the mother liquor of the copper-containing wastewater is 1.1:1, and the control drop-added temperature does not exceed 50 °C;

[0042] S3, after the drop addition, after adding copper hydroxide stirred for 1h found not completely dissolved, at this time slowly add concentrated sulfuric acid, until completely dissolved, the control temperature in the process does not exceed 50 °C, the quality of copper hydroxide is 2.5 times the concentrated sulfuric acid in the step S2;

[0043] S4, add activated carbon stirring for 2h, the control temperature in the process does not exceed 50 °C, after t...

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Abstract

The invention relates to the technical field of waste liquid treatment, and provides a copper sulfate recovery treatment process in a methyl o-formate benzenesulfonamide production process, which comprises the following steps: S1, adding alkali into copper-containing wastewater mother liquor for neutralization treatment, and then carrying out filter pressing to prepare copper hydroxide; s2, dissolving the copper hydroxide obtained in the step S1 into water, slowly dropwise adding concentrated sulfuric acid, and controlling the dropwise adding temperature not to exceed 50 DEG C; s3, after dropwise adding, supplementing the copper hydroxide until the copper hydroxide is completely dissolved; s4, adding activated carbon, stirring for 1-2 hours, and directly performing suction filtration after stirring is finished; s5, distilling and concentrating the filtrate; and S6, centrifuging the distilled and concentrated copper sulfate solution to obtain recovered copper sulfate.

Description

Technical field [0001] The present invention relates to the field of waste liquid treatment technology, specifically, relates to a copper sulfate recovery process in the production process of methyl o-formate benzene sulfonamide. Background [0002] In the process of preparing methyl oformate benzene sulfonamide with phthalic anhydride as raw material, amidation, Hoffmann degradation, diazo, displacement, chlorination, amination and other processes, there is a process that uses copper sulfate as a catalyst, diazo salt and sulfur dioxide to produce methyl phenenylene sulfinate o-carboxylate. In this project, due to the use of copper sulfate as a catalyst, the resulting mother liquor is containing copper sulfate, if not recycled will cause a lot of waste, increase the cost, but there is no current application to the production process of methyl formate benzene sulfonamide containing copper waste liquid to recover copper sulfate. Contents of the Invention [0003] The present inven...

Claims

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Application Information

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IPC IPC(8): C01G3/10
CPCC01G3/10C01G3/003C01P2006/80
Inventor 蒲帅天赵英福张金峰
Owner 河北允升精细化工有限公司
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