CN105540923A - Method for removing 2-mercaptopyridine-N-oxide in wastewater and recycling of 2-mercaptopyridine-N-oxide - Google Patents
Method for removing 2-mercaptopyridine-N-oxide in wastewater and recycling of 2-mercaptopyridine-N-oxide Download PDFInfo
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- CN105540923A CN105540923A CN201510989031.9A CN201510989031A CN105540923A CN 105540923 A CN105540923 A CN 105540923A CN 201510989031 A CN201510989031 A CN 201510989031A CN 105540923 A CN105540923 A CN 105540923A
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- pyrithione
- waste water
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- organic solvent
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- OKDGRDCXVWSXDC-UHFFFAOYSA-N Clc1ncccc1 Chemical compound Clc1ncccc1 OKDGRDCXVWSXDC-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
Abstract
The invention discloses a method for removing 2-mercaptopyridine-N-oxide in wastewater and recycling of the 2-mercaptopyridine-N-oxide. The method comprises the following steps: (1) mixing the wastewater containing the 2-mercaptopyridine-N-oxide and an organic solvent at a room temperature according to a ratio of (7:1) to (12:1); after stirring for 1 to 2 hours, standing for 0.5 to 1 hour; layering and separating and removing a wastewater layer; determining that the content of the 2-mercaptopyridine-N-oxide in the separated and removed wastewater layer is less than 0.05 percent; (2) at the room temperature, adding de-ionized water into the organic solvent layered by the step (1); stirring and dropwise adding a sodium hydroxide solution with the mass concentration of 30 percent until the pH value of the mixed solution is 9 to 10; continually stirring for 0.5 to 1 hour; then standing for 0.5 to 1 hour and layering. With the adoption of the method disclosed by the invention, the content of the 2-mercaptopyridine-N-oxide in the wastewater is effectively reduced, the chroma and suspended matters of the wastewater are reduced, and convenience for treating three wastes is brought.
Description
Technical field
The invention belongs to chemical field, particularly relate to a kind of method and recycling thereof of removing pyrithione in waste water.
Background technology
Pyrithione is slightly soluble in water, be soluble in highly basic, be dissolved in the organic solvents such as halohydrocarbon, aromatic hydrocarbon, ether and ester, for the preparation of various pyrithione, and pyrithione is widely used in the field such as daily washing cosmetic and paint of coating industry as sterilant.The preparation of pyrithione in current industrial production, generally with 2-chloropyridine for starting raw material, through hydrogen peroxide oxidation, mercaptolation obtain, concrete technology synthetic route is as follows:
In actual production, 2-chloropyridine is after oxidation, sulfhydrylation obtain pyrithione sodium salt, pyrithione sodium salt need adjust pH to 2-3 with hydrochloric acid or sulfuric acid, separate out pyrithione solid, filter the pyrithione solid repeated hydrogenation sodium hydroxide solution obtained to dissolve, obtained pyrithione sodium salt solution, then go to prepare various pyrithione, this acid out and the molten process of alkali are purification process, and object improves pyrithione sodium salt quality.
Present problem is after the pyrithione solid filtering of acid out, the pyrithione of still residual 0.3-0.4% in the waste water of generation, pH value when how many its residual quantities depends primarily on filtration and filtration temperature etc.Because pyrithione itself is not very stable, long-time chance light and heat meeting variable color, also other compound easily and in other waste water reacts, so, certain colourity and turbidity can be produced containing pyrithione concentration height in waste water, directly enter wastewater treatment equipment, waste water can be made to be difficult to process, and, pyrithione is a sterilant, restraining effect is had to the microorganism of wastewater biochemical process, according to our practical experience, the waste water produced after filtering comparatively is beneficial to wastewater biochemical process containing pyrithione content below 0.05%.
How the waste water of the pyrithione containing 0.3-0.4% is removed and utilize pyrithione, have no bibliographical information at present, usually can add zinc sulfate or copper sulfate to produce Zinc Pyrithione (copper) precipitation and remove pyrithione in waste water, but Zinc Pyrithione (copper) content reclaimed is low, needing purifies further could effectively utilize, and can produce new pollution.Like this, we need seek removing and the Application way of new pyrithione.
Summary of the invention
The present invention seeks to for the deficiencies in the prior art, a kind of method and recycling thereof of removing pyrithione in waste water are provided.
The technical solution adopted for the present invention to solve the technical problems step is as follows:
Step (1). at room temperature, the waste water containing pyrithione is mixed with organic solvent in certain ratio, stirs after 1-2 hour, leave standstill 0.5-1 hour, layering, divide except waste water layer.After measured, in point waste water layer removed, pyrithione content is less than 0.05%, and point waste water removed is placed in Waste Water Treatment.
The blending ratio containing pyrithione waste water and organic solvent mentioned in described step (1) is 7:1-12:1.
Described organic solvent comprises toluene and the Mixed XYLENE of arene, the methylene dichloride of halogenated hydrocarbon, trichloromethane and 1,2-methylene dichloride, the ethyl acetate of ester class, methyl acetate and ethyl formate, the methyl tertiary butyl ether of ethers and isopropyl ether;
The preferred toluene of described organic solvent and methyl tertiary butyl ether.
The pH value containing pyrithione waste water mentioned in described step (1) is 2-6.
Step (2). at room temperature, deionized water is added in the organic solvent after step (1) layering, then dripping mass concentration is while stirring the sodium hydroxide solution of 30%, until the pH value of mixing solutions is 9-10, continue to stir after 0.5-1 hour and leave standstill 0.5-1 hour, layering, the water layer separated is pyrithione sodium salt solution, and the content of pyrithione sodium salt is 35-41% in water layer, this water layer can be used in production pyrithione.
Organic solvent layer in described step (2) after layering can be used in removing and the recycling thereof of pyrithione in next batch waste water after benefit amount.
The deionized water mentioned in described step (2) and the mass ratio of waste water are 1:300-500.
Beneficial effect of the present invention is as follows:
The present invention not only effectively reduces the content of pyrithione in waste water, and the colourity of waste water and suspended substance are reduced, for three-protection design offers convenience, and the pyrithione sodium salt reclaimed can be used for production pyrithione, brings certain economic benefit.
If in pyrithione sodium salt production process, the pyrithione that acid out goes out does not filter, directly with organic solvent extraction, this can consume a large amount of organic solvent, increase production cost and safety in production hidden danger, and can increase the risk of residual a large amount of organic solvent in the finished product pyrithione.And the present invention makes whole technique environmental protection.
Embodiment
Below in conjunction with example, the invention will be further described.
Embodiment 1
In the glass reaction bottle of 5L, add 0.5 ㎏ toluene, add pH value be adjusted in advance 3-4 containing pyrithione waste water 4.5 ㎏, at room temperature stir 1 hour, sampling of wastewater is analyzed, and at this moment containing pyrithione in waste water is 0.042%, leaves standstill 0.5 hour, layering, separates waste water layer.
Layering is complete, adds 0.01 ㎏ deionized water, and dripping 30% sodium hydroxide solution 0.015 ㎏, is 9 to pH value, stirs 0.5 hour, leaves standstill 0.5 hour, layering, and point water-yielding stratum 0.039 ㎏, its pyrithione sodium salt content is 40.3%.
Embodiment 2
In the glass reaction bottle of 5L, add 0.6 ㎏ methylene dichloride, add pH value be 2-3 containing pyrithione waste water 4.5 ㎏, at room temperature stir 1 hour, sampling of wastewater is analyzed, and containing pyrithione in waste water is 0.033%, leaves standstill 0.5 hour, layering, separates waste water layer.
Layering is complete, adds 0.015 ㎏ deionized water, and dripping 30% sodium hydroxide solution 0.016 ㎏, is 9 to pH value, stirs 0.5 hour, leaves standstill 0.5 hour, layering, and point water-yielding stratum 0.046 ㎏, its pyrithione sodium salt content is 35.5%.
Embodiment 3
In the glass reaction bottle of 5L, add 0.5 ㎏ methyl tertiary butyl ether, add pH value be adjusted in advance 4-5 containing pyrithione waste water 4.5 ㎏, at room temperature stir 1 hour, sampling of wastewater is analyzed, and containing pyrithione in waste water is 0.038%, leaves standstill 0.5 hour, layering, separates waste water layer.
Layering is complete, adds 0.01 ㎏ deionized water, and dripping 30% sodium hydroxide solution 0.015 ㎏, is 9 to pH value, stirs 0.5 hour, leaves standstill 0.5 hour, layering, and point water-yielding stratum 0.04 ㎏, its pyrithione sodium salt content is 40.2%.
Embodiment 4
In the glass reaction bottle of 5L, add 0.4 ㎏ methyl tertiary butyl ether, add pH value be adjusted in advance 4-5 containing pyrithione waste water 4.5 ㎏, at room temperature stir 2 hours, sampling of wastewater is analyzed, and containing pyrithione in waste water is 0.04%, leaves standstill 1 hour, layering, separates waste water layer.
Layering is complete, adds 0.009 ㎏ deionized water, and dripping 30% sodium hydroxide solution 0.015 ㎏, is 10 to pH value, stirs 0.5 hour, leaves standstill 0.5 hour, layering, and point water-yielding stratum 0.038 ㎏, its pyrithione sodium salt content is 41.0%.
Embodiment 5
In the glass reaction bottle of 5L, add 0.5 ㎏ ethyl acetate, add pH value be adjusted in advance 5-6 containing pyrithione waste water 4.5 ㎏, at room temperature stir 1 hour, sampling of wastewater is analyzed, and containing pyrithione in waste water is 0.041%, leaves standstill 0.5 hour, layering, separates waste water layer.
Layering is complete, adds 0.01 ㎏ deionized water, and dripping 30% sodium hydroxide solution 0.017 ㎏, is 9 to pH value, stirs 0.5 hour, leaves standstill 0.5 hour, layering, and point water-yielding stratum 0.042 ㎏, its pyrithione sodium salt content is 38.8%.
Embodiment 6
In the glass reaction bottle of 5L, add 0.45 ㎏ methyl acetate, add pH value be adjusted in advance 5-6 containing pyrithione waste water 4.5 ㎏, at room temperature stir 1 hour, sampling of wastewater is analyzed, and containing pyrithione in waste water is 0.042%, leaves standstill 0.5 hour, layering, separates waste water layer.
Layering is complete, adds 0.01 ㎏ deionized water, and dripping 30% sodium hydroxide solution 0.016 ㎏, is 9 to pH value, stirs 0.5 hour, leaves standstill 0.5 hour, layering, and point water-yielding stratum 0.041 ㎏, its pyrithione sodium salt content is 39.1%.
Embodiment 7
In the glass reaction bottle of 5L, add 3.75 ㎏ ethyl formates, add pH value be adjusted in advance 5-6 containing pyrithione waste water 4.5 ㎏, at room temperature stir 1 hour, sampling of wastewater is analyzed, and containing pyrithione in waste water is 0.046%, leaves standstill 0.5 hour, layering, separates waste water layer.
Layering is complete, adds 0.01 ㎏ deionized water, and dripping 30% sodium hydroxide solution 0.016 ㎏, is 9 to pH value, stirs 0.5 hour, leaves standstill 0.5 hour, layering, and point water-yielding stratum 0.038 ㎏, its pyrithione sodium salt content is 39.3%.
Embodiment 8
In the glass reaction bottle of 5L, add 0.643 ㎏ trichloromethane, add pH value be 2-3 containing pyrithione waste water 4.5 ㎏, at room temperature stir 1 hour, sampling of wastewater is analyzed, and containing pyrithione in waste water is 0.03%, leaves standstill 0.5 hour, layering, separates waste water layer.
Layering is complete, adds 0.015 ㎏ deionized water, and dripping 30% sodium hydroxide solution 0.016 ㎏, is 9 to pH value, stirs 0.5 hour, leaves standstill 0.5 hour, layering, and point water-yielding stratum 0.046 ㎏, its pyrithione sodium salt content is 36.7%.
Embodiment 9
In the glass reaction bottle of 5L, add 0.6 ㎏ 1,2-ethylene dichloride, add pH value be 2-3 containing pyrithione waste water 4.5 ㎏, at room temperature stir 1 hour, sampling of wastewater analysis, containing pyrithione in waste water is 0.034%, leave standstill 0.5 hour, layering, separates waste water layer.
Layering is complete, adds 0.015 ㎏ deionized water, and dripping 30% sodium hydroxide solution 0.016 ㎏, is 9 to pH value, stirs 0.5 hour, leaves standstill 0.5 hour, layering, and point water-yielding stratum 0.047 ㎏, its pyrithione sodium salt content is 35.1%.
Embodiment 10
In the glass reaction bottle of 5L, add 0.55 ㎏ Mixed XYLENE, add pH value be adjusted in advance 3-4 containing pyrithione waste water 4.5 ㎏, at room temperature stir 1 hour, sampling of wastewater is analyzed, and at this moment containing pyrithione in waste water is 0.043%, leaves standstill 0.5 hour, layering, separates waste water layer.
Layering is complete, adds 0.01 ㎏ deionized water, and dripping 30% sodium hydroxide solution 0.015 ㎏, is 9 to pH value, stirs 0.5 hour, leaves standstill 0.5 hour, layering, and point water-yielding stratum 0.04 ㎏, its pyrithione sodium salt content is 40.2%.
Embodiment 11
In the glass reaction bottle of 5L, add 0.45 ㎏ isopropyl ether, add pH value be adjusted in advance 4-5 containing pyrithione waste water 4.5 ㎏, at room temperature stir 1 hour, sampling of wastewater is analyzed, and containing pyrithione in waste water is 0.039%, leaves standstill 0.5 hour, layering, separates waste water layer.
Layering is complete, adds 0.01 ㎏ deionized water, and dripping 30% sodium hydroxide solution 0.015 ㎏, is 9 to pH value, stirs 0.5 hour, leaves standstill 0.5 hour, layering, and point water-yielding stratum 0.039 ㎏, its pyrithione sodium salt content is 40.5%.
Embodiment 12:
In the reactor of 5000L, add 500 ㎏ toluene, with pump squeeze into pH value 2-3 containing pyrithione waste water 4500 ㎏, at room temperature stir 1 hour, sampling of wastewater is analyzed, and containing pyrithione in waste water is 0.044%, leaves standstill 1 hour, layering, the waste water separated removes Waste Water Treatment.
Layering is complete, adds 10 ㎏ deionized waters, and dripping 30% sodium hydroxide solution 15 ㎏, is 9 to pH value, stirs 0.5 hour, leaves standstill 1 hour, layering, and divide water-yielding stratum barrelling, be weighed as 40 ㎏, its content is 39.5%.After this pyrithione sodium salt solution is concentrated, for the production of pyrithione.Toluene still in a kettle., after suitable benefit amount, for removing and the utilization of pyrithione in lower batch of waste water.
Embodiment 13:
In the reactor of the 5000L of embodiment 12, add 10 ㎏ toluene, with pump squeeze into pH value be adjusted in advance 4-5 containing pyrithione waste water 4500 ㎏, at room temperature stir 1 hour, sampling of wastewater is analyzed, and pyrithione contained by waste water is 0.041%, leaves standstill 1 hour, layering, the waste water separated removes Waste Water Treatment.
Layering is complete, adds 10 ㎏ deionized waters, and dripping 30% sodium hydroxide solution 15 ㎏, is 10 to pH value, stirs 0.5 hour, leaves standstill 1 hour, layering, and divide water-yielding stratum barrelling, be weighed as 39.8 ㎏, its content is 39.9%.After this pyrithione sodium salt solution is concentrated, for the production of pyrithione.Toluene still in a kettle., after suitable benefit amount, for removing and the utilization of pyrithione in lower batch of waste water.
Claims (5)
1. remove method and the recycling thereof of pyrithione in waste water, it is characterized in that comprising the steps:
Step (1). at room temperature, the waste water containing pyrithione is mixed with organic solvent in certain ratio, stirs after 1-2 hour, leave standstill 0.5-1 hour, layering, divide except waste water layer; After measured, in point waste water layer removed, pyrithione content is less than 0.05%, and point waste water removed is placed in Waste Water Treatment;
The blending ratio containing pyrithione waste water and organic solvent mentioned in described step (1) is 7:1-12:1;
Described organic solvent comprises toluene and the Mixed XYLENE of arene, the methylene dichloride of halogenated hydrocarbon, trichloromethane and 1,2-methylene dichloride, the ethyl acetate of ester class, methyl acetate and ethyl formate, the methyl tertiary butyl ether of ethers and isopropyl ether;
Step (2). at room temperature, deionized water is added in the organic solvent after step (1) layering, then dripping mass concentration is while stirring the sodium hydroxide solution of 30%, until the pH value of mixing solutions is 9-10, continue to stir after 0.5-1 hour and leave standstill 0.5-1 hour, layering, the water layer separated is pyrithione sodium salt solution, and the content of pyrithione sodium salt is 35-41% in water layer, this water layer can be used in production pyrithione;
The deionized water mentioned in described step (2) and the mass ratio of waste water are 1:300-500.
2. a kind of method and recycling thereof of removing pyrithione in waste water as claimed in claim 1, is characterized in that the organic solvent described in step (1) is toluene and methyl tertiary butyl ether.
3. a kind of method and recycling thereof of removing pyrithione in waste water as claimed in claim 1, is characterized in that the pH value containing pyrithione waste water mentioned in described step (1) is 2-6.
4. a kind of method and recycling thereof of removing pyrithione in waste water as claimed in claim 1, is characterized in that the organic solvent layer in described step (2) after layering can be used in the removing of pyrithione in next batch waste water after benefit amount.
5. a kind of method and recycling thereof of removing pyrithione in waste water as claimed in claim 1, it is characterized in that the water layer separated in described step (2) is pyrithione sodium salt solution, and the content of pyrithione sodium salt is 35-41% in water layer, this water layer can be used in production pyrithione.
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| CN108439646A (en) * | 2018-04-17 | 2018-08-24 | 中南大学 | A kind of preprocess method of organic wastewater with high concentration during sulfhydryl heterocycle class production of chemicals |
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| CN105540923B (en) | 2017-12-12 |
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