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Process of recycling mother liquor waste water in naphthol production

A production process and waste water recycling technology, applied in the preparation of organic compounds, organic chemistry, chemical instruments and methods, etc., can solve the problems of staggering costs, waste of resources, increased consumption of extractants, acids, and alkalis, etc.

Active Publication Date: 2022-04-15
孙骜 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

"The main problem here is that the valuable naphthalenesulfonate in the mother liquor is oxidized and wasted, and the valuable sodium sulfite and sodium bisulfite are also oxidized into sodium sulfate with very low added value, wasting resources
[0007] In the above-mentioned treatment method of mother liquor wastewater, the valuable naphthalenesulfonate and sulfite in the mother liquor wastewater are partially or completely wasted, and some also increase the consumption of extractant, acid and alkali, resulting in great waste
Moreover, the final solid waste needs further harmless treatment, and the cost is astonishing
[0008] The existing method is to post-treat the mother liquor wastewater, which does not fully consider the comprehensive utilization of the mother liquor wastewater.
However, the treatment method of sodium sulfite "wastewater" originally used evaporation crystallization or boiling granulation to recover sodium sulfite, which has high recovery costs and secondary pollution.
The sodium sulfite recovery method disclosed in "Patent ZL200610016781.9" greatly reduces the recovery cost of sodium sulfite. This patent has certain limitations for the treatment of mother liquor wastewater

Method used

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  • Process of recycling mother liquor waste water in naphthol production
  • Process of recycling mother liquor waste water in naphthol production

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Embodiment 1 (taking 2-naphthol production as example)

[0026] Refined naphthalene and concentrated sulfuric acid are mixed in a certain proportion, sulfonated at 164°C to form naphthalene sulfonate, and then neutralized by adding an appropriate amount of alkali (to neutralize excess sulfuric acid) after naphthalene blowing (recovering unreacted naphthalene) The former material (referred to as the former material, the main component is naphthalenesulfonic acid), and then sent to the neutralization process. In the neutralization process, gradually add an appropriate amount of neutralizing agent at 90°C (the neutralizing agent prepared by extracting the mother liquor, wherein the concentration of sodium sulfite is 170g / L) to the right point to generate SO 2 Deacidification. The neutralized substance is cooled to 40°C with indirect water, and then the naphthalenesulfonate and the neutralization mother liquor are separated through a vacuum filtration system, and the drain...

Embodiment 2

[0028] Embodiment 2 (taking 2-naphthol production as example)

[0029] Take 1 part of the sulfonated product of the sulfonated alkali fusion method, and gradually add a 90°C neutralizer at 130°C (from the neutralizer storage tank of the system, with a sodium sulfite concentration of 170g / L), and neutralize to the point where the generated sulfur dioxide is removed. acidification. The neutralized product is cooled to 40°C, and the cooled product is filtered (solid-liquid separation) to obtain naphthalenesulfonate and sent to the alkali melting silo; the filtered mother liquid (neutralized mother liquid) is evaporated to concentrate about 60% of the original liquid, and gradually cooled to 35 ℃, filter and recover naphthalene sulfonate (alkali melting silo); the secondary mother liquor separated by filtration continues to be cooled to 20 ℃, and then filtered to separate solid sodium sulfate, that is, Glauber's salt, and the filtrate is the extraction mother liquor. Extract the ...

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Abstract

The invention provides a process for recycling mother liquor wastewater in naphthol production, the mother liquor wastewater in naphthol production, the extracted mother liquor after extracting part of the sulfate, or the extracted mother liquor after extracting part of the naphthalenesulfonate and part of the sulfate , directly or indirectly return to the production process system for neutralization reaction. The extracted mother liquor is directly returned to the production process system for neutralization reaction, or sodium sulfite is added to the extracted mother liquor to prepare a neutralizing agent and then returned to the production process system for neutralization reaction. Beneficial effects of the present invention: (1) The mother liquor wastewater is recirculated, with little or no discharge, completely solving the problem that the mother liquor wastewater produced by naphthol is difficult to treat. (2) Recover and utilize the valuable naphthalene sulfonate and sulfite in the mother liquor, and greatly reduce the unit consumption of refined naphthalene, acid and alkali.

Description

technical field [0001] The present invention relates to a kind of technology of mother liquor waste water recycling in the production of naphthol, namely the process method of the mother liquor waste water recycling that the naphthol (comprising 1-naphthol and 2-naphthol) production of sulfonated alkali fusion method produces, also is Cleaner production process for naphthol production. Background technique [0002] At present, the production of naphthol (1-naphthol and 2-naphthol) in my country is mainly sulfonated alkali fusion method, and its production process is: refined naphthalene is obtained by sulfonation, neutralization, cooling and crystallization, and solid-liquid separation Salt, naphthalene sulfonate alkali fusion, dilution, acidification, boiling separation, dry distillation (or re-distillation), crystal slice packaging to obtain naphthol products. This process produces two major process "wastewater", one is the filtrate after the neutralization product is cool...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C37/04C07C39/14
Inventor 孙骜李阳
Owner 孙骜
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