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Process for producing H acid by recycling alkali fusion mother liquor

A technology of alkali fusion and mother liquor, which is applied in the preparation of sulfonic acid and organic chemistry, and can solve the problems of large amount of potassium hydroxide and unfavorable production costs

Active Publication Date: 2018-12-28
SHANDONG CHUANGLAN YAOSHI ENVIRONMENTAL PROTECTION TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the previous research of the present invention (Patent No. ZL201410816923.4), potassium hydroxide was used instead of traditional ammonia water as a neutralizing solution to produce nitro-T acid, and potassium hydroxide was used instead of sodium hydroxide alkali fusion to generate potassium sulfate mother liquor through MVR Concentrated crystallization and high-temperature calcination to produce potassium sulfate completely solved the environmental protection problems that plagued enterprises, and at the same time improved the yield of the product, but the disadvantage of this method is that the amount of potassium hydroxide is too large, and 48% of H acid product is consumed per ton More than 11 tons of potassium hydroxide are unfavorable for controlling the production cost of the product. Based on this problem, the present invention further studies a process for producing H acid by recycling the alkali-melted mother liquor, in order to reduce the production cost on the basis of ensuring cleanliness and environmental protection. Production cost of H acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] A kind of technology that produces H acid by mother liquor recycling, comprises the steps:

[0061] (1) get refined naphthalene through traditional process sulfonation, nitration, 400 parts (weight parts, the same below) of the nitro-T acid reaction solution that obtains through traditional process sulfonation, nitration, denitrification, get and contain 560 parts of alkali fusion mother liquors of potassium sulfite 45% and nitro-T The acid reaction solution is neutralized, and the sulfur dioxide generated during the neutralization reaction is removed at 80-100°C for 1 hour, and then the reaction solution is lowered to room temperature, crystallized, and filtered to obtain a nitrotrate solid and filtrate, which are set aside ; Sulfur dioxide is collected centrally for backup;

[0062] (2) Get 250 parts of potassium sulfite alkali fusion mother liquor whose mass concentration is 45%, continue to neutralize with the filtrate produced in step (1), and remove the sulfur dio...

Embodiment 2

[0068] A kind of technology that produces H acid by mother liquor recycling, comprises the steps:

[0069] (1) get refined naphthalene through traditional process sulfonation, nitration, 1000 parts (weight parts, the same below) of the nitro-T acid reaction solution that obtains through traditional process sulfonation, nitration, denitrification, react with 1200 parts of 40% alkali fusion mother liquors containing sodium sulfite concentration and nitro-T acid neutralize the reaction solution, and remove the sulfur dioxide produced during the neutralization reaction at 80-100°C for 3 hours, then lower the reaction solution to room temperature, crystallize, and filter to obtain the nitrotrate solid and filtrate for subsequent use; sulfur dioxide Centralized collection, standby;

[0070] (2) Take 600 parts of sodium sulfite alkali fusion mother liquor whose mass concentration is 40%, continue to neutralize with the filtrate produced in step (1), and remove the sulfur dioxide 3h p...

Embodiment 3

[0076] A kind of technology that produces H acid by mother liquor recycling, comprises the steps:

[0077] (1) get refined naphthalene through traditional process sulfonation, nitration, 400 parts (weight parts, the same below) of the nitro-T acid reaction solution that obtains through traditional process sulfonation, nitration, denitrification, get and contain 560 parts of alkali fusion mother liquors of potassium sulfite 45% and nitro-T The acid reaction solution is neutralized, and the sulfur dioxide generated during the neutralization reaction is removed at 80-100°C for 1 hour, and then the reaction solution is lowered to room temperature, crystallized, and filtered to obtain a nitrotrate solid and filtrate, which are set aside ; Sulfur dioxide is collected centrally for backup;

[0078] (2) Get 300 parts of lightly burned magnesium powder, continue to neutralize with the filtrate produced in the step (1), then cool down, crystallize, filter to obtain the magnesium sulfate...

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Abstract

The invention relates to a process for producing H acid by recycling alkali fusion mother liquor, and belongs to the technical field of preparation for the H acid. According to the invention, sulfiteis used to replace potassium hydroxide or sodium hydroxide and is used as a neutralization solution of a denitrification reaction solution, and can be continuously recycled in the process of preparingthe H acid, so that the use amount of potassium hydroxide of which the concentration is 48% is reduced from 11 tons of the original process to less than 5 tons, and the use amount of sodium hydroxideof which the concentration is 48% is reduced from 8 tons originally to less than 3.5 tons, so that the consumption of potassium hydroxide or sodium hydroxide is greatly lowered to effectively lower the production cost of the product.

Description

technical field [0001] The invention relates to the technical field of preparation of H acid, in particular to a process for producing H acid by continuously recycling mother liquor. Background technique [0002] H acid (monosodium 1-amino-8-naphthol-3,6-disulfonate) is an important intermediate in the production of reactive dyes. At present, the production of H acid uses refined naphthalene as a raw material, and amino T acid is first prepared through sulfonation, nitration, denitrification, neutralization, reduction, sodium chloride salting out and other processes, and amino T acid is then subjected to alkali melting and acidification. Production of H acid, however, the mother liquor produced during the production of H acid belongs to the "five high" organic wastewater with high concentration, high acidity, high salinity, high chroma, and high toxicity, and the chemical oxygen demand (Chemical OxygenDemand-COD) is as high as 80,000 to 100,000, the salt content is as high ...

Claims

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Application Information

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IPC IPC(8): C07C309/50C07C303/22
CPCC07C303/22C07C309/40C07C309/47C07C309/50
Inventor 王在军张克宏任帅昌杨海军石艳
Owner SHANDONG CHUANGLAN YAOSHI ENVIRONMENTAL PROTECTION TECH CO LTD
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