CN114506896A - Application of n-nonanol in separation of emulsified oil in coal chemical oil-containing wastewater and method - Google Patents
Application of n-nonanol in separation of emulsified oil in coal chemical oil-containing wastewater and method Download PDFInfo
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- CN114506896A CN114506896A CN202210098469.8A CN202210098469A CN114506896A CN 114506896 A CN114506896 A CN 114506896A CN 202210098469 A CN202210098469 A CN 202210098469A CN 114506896 A CN114506896 A CN 114506896A
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/02—Temperature
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2209/06—Controlling or monitoring parameters in water treatment pH
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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
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Abstract
The invention belongs to the technical field of sewage treatment, and particularly relates to application of n-nonanol in separation of emulsified oil in coal chemical oil-containing wastewater and a method thereof. The method comprises the following steps: the method takes n-nonanol as an extracting agent to carry out multi-stage cross-flow extraction on the coal chemical industry oily wastewater, thereby realizing the separation of emulsified oil in the coal chemical industry oily wastewater. The method for separating the emulsified oil from the oily wastewater in the coal chemical industry has obvious deoiling effect on the emulsified oil in the oily wastewater in the coal chemical industry, and the removal rate of the emulsified oil is more than 96 percent. Moreover, since n-nonanol is practically insoluble in water, the process of the invention does not require additional energy application such as stripping, and allows the extractant residual in the raffinate phase to be controlled below 100 mg/L. In addition, the method is favorable for solving a series of problems caused by tar blockage and scaling of a subsequent phenol-ammonia recovery device.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to application of n-nonanol in separation of emulsified oil in coal chemical oil-containing wastewater and a method thereof.
Background
The semi-coke wastewater is obtained from the low-temperature carbonization (500-800 ℃) process of coal. The waste water has high oil content, a large amount of tar is dispersed in water in the form of emulsified oil under the action of surface active substances such as micro coal powder, coke powder, asphaltene, organic acid and the like, and the particle size of oil drops is less than 5 microns. In the prior art, the salt content in the wastewater is increased due to the addition of medicaments, such as an air flotation method, a flocculation sedimentation method and the like, so that the treatment load of the subsequent desalting process is increased. Most importantly, these methods have limitations in handling emulsified oil and the de-oiling effect is not ideal. At present, actual operation data of most semi-coke plants show that the oil content in inlet water of a subsequent phenol ammonia recovery device exceeds 500mg/L, even reaches 1000 mg/L. A large amount of tar enters the phenol ammonia recovery device, so that scaling and blockage of a tower tray and a heat exchanger of the device are caused, the mass transfer and heat transfer efficiency is reduced, and the continuous stable operation and pollutant treatment effect of the device are influenced.
Therefore, it is urgently needed to develop a method for treating the oily wastewater in the coal chemical industry, which has a good emulsified oil removal effect and does not cause secondary pollution.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention mainly aims to provide the application of n-nonanol in separation of emulsified oil in coal chemical industry oil-containing wastewater.
The invention also aims to provide a method for separating emulsified oil from oily wastewater in coal chemical industry.
The purpose of the invention is realized by the following technical scheme:
the extraction is to transfer the substance from one solvent to another by using the different solubility of the substance in the immiscible solvents, and the method has no secondary pollution and no damage to the waste water treatment system. The invention provides application of n-nonanol as an extracting agent in separation of emulsified oil in coal chemical industry oil-containing wastewater. The inventor finds that n-nonanol has a high distribution coefficient for emulsified oil in coal chemical industry oily wastewater in experiments, and is almost insoluble in water, so that when the n-nonanol is used for separating the emulsified oil in coal chemical industry oily wastewater, the deoiling effect is obvious.
The invention also provides a method for separating emulsified oil from the oily wastewater in the coal chemical industry, which comprises the following steps: the method takes n-nonanol as an extracting agent to carry out multi-stage cross-flow extraction on the coal chemical industry oily wastewater, thereby realizing the separation of emulsified oil in the coal chemical industry oily wastewater.
Preferably, the content of emulsified oil in the oily wastewater in the coal chemical industry is 500 mg/L-2000 mg/L.
Preferably, the volume ratio of the n-nonanol to the coal chemical oil-containing wastewater is 1 (2-7).
Preferably, the coal chemical oil-containing wastewater is semi-coke wastewater.
Preferably, the emulsified oil in the oily wastewater in the coal chemical industry is emulsified oil containing a naphthalene compound.
Preferably, the multistage cross-flow extraction is carried out under the condition that the pH value is 6-12; more preferably, the extraction is carried out at a pH of 6 to 9.
Preferably, the multistage cross-flow extraction is carried out at the temperature of 20-70 ℃; more preferably, the extraction is carried out at a temperature of 20 to 40 ℃.
Preferably, in the multi-stage cross-flow extraction process, the stirring time of each stage of extraction is 30-60 min, and the standing phase separation time is 30-60 min.
Preferably, after the multistage cross-flow extraction, a hydrocyclone is adopted to accelerate partial emulsified oil in the extraction phase to gather and separate from the extraction phase.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the method for separating the emulsified oil from the oily wastewater in the coal chemical industry has obvious deoiling effect on the emulsified oil in the oily wastewater in the coal chemical industry, and the removal rate of the emulsified oil is more than 96 percent.
(2) Because the n-nonanol is almost insoluble in water, the method for separating the emulsified oil from the oily wastewater in the coal chemical industry does not need additional energy application such as steam stripping, and the residual amount of the extractant in the raffinate phase can be controlled below 100 mg/L.
(3) The invention provides a method for solving emulsified oil in oily wastewater in coal chemical industry, which is beneficial to solving a series of problems caused by tar blockage and scaling of a subsequent phenol-ammonia recovery device.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. The raw materials related to the invention can be directly purchased from the market. For process parameters not specifically noted, reference may be made to conventional techniques.
The polycyclic aromatic hydrocarbon compound is the main component of oil substances in the semi-coke wastewater and accounts for more than 90 percent of the total amount of pollutants. Wherein the naphthalene compound has significant content in the polycyclic aromatic hydrocarbon, and accounts for more than 60% of the total amount of the polycyclic aromatic hydrocarbon. Sodium dodecyl sulfate is easily dissolved in water, has a density close to that of water, and is a commonly used emulsifier, so in the following examples 1-11, sodium dodecyl sulfate is selected as a surface active substance, and 1-methylnaphthalene, 1-ethylnaphthalene, 2-methylbiphenyl, and 2-methylacenaphthylene are respectively used as characteristic pollutants to prepare emulsified oil wastewater to simulate coal chemical industry oily wastewater for experiments.
The 1-methylnaphthalene, 2-ethylnaphthalene emulsified oil content of the following examples was determined by the following method: analysis of each component was performed using a liquid chromatograph using a 250mm 4.6mm 5um Agilent chromatography column and an ultraviolet absorption detector. The mobile phase comprises acetonitrile solution and 0.5% acetic acid water solution, and the volume ratio of the acetonitrile solution to the 0.45: 0.55, flow rate of 0.8ml/min, data acquisition time of 60min, wavelength of light used by the ultraviolet detector of 270nm, and column oven of 35 ℃.
The following 2-methylbiphenyl emulsified oil content was determined by the following method: analysis of each component was performed using a liquid chromatograph using a 250mm 4.6mm 5um Agilent chromatography column and an ultraviolet absorption detector. The mobile phase comprises acetonitrile solution and 0.5% acetic acid water solution, and the volume ratio of the acetonitrile solution to the 0.5% acetic acid water solution is: 0.5, the flow rate is 0.8ml/min, the data acquisition time is 60min, the wavelength of light used by the ultraviolet detector is 280nm, and the column oven is 35 ℃.
The following 2-methylacenaphthylene emulsified oil content was measured by the following method: analysis of each component was performed using a liquid chromatograph using a 250mm 4.6mm 5um Agilent chromatography column and an ultraviolet absorption detector. The mobile phase comprises acetonitrile solution and 0.5% acetic acid water solution, and the volume ratio of the acetonitrile solution to the 0.5% acetic acid water solution is 0.6: 0.4, the flow rate is 0.8ml/min, the data acquisition time is 60min, the wavelength of light used by the ultraviolet detector is 260nm, and the column incubator is 35 ℃.
In examples 1 to 11, sodium dodecyl sulfate was selected as a surface active substance, and 1-methylnaphthalene, 1-ethylnaphthalene, 2-methylbiphenyl, and 2-methylacenaphthylene were respectively used as characteristic contaminants to prepare emulsified oil-containing wastewater (hereinafter referred to as emulsified oil wastewater) stabilized with sodium dodecyl sulfate for simulation of coal chemical industry, and the experimental procedures were as follows: and (2) taking n-nonanol as an extracting agent, performing multistage cross-flow extraction on the emulsified oil wastewater, and separating the emulsified oil in the emulsified oil wastewater to obtain the wastewater after extraction treatment.
Example 1
The emulsified oil wastewater with the emulsified oil content of 1951mg/L of 1-methylnaphthalene is treated in the embodiment, and the emulsified oil wastewater and n-nonanol are mixed according to the volume ratio of 5:1, carrying out secondary cross-flow extraction; extraction conditions are as follows: controlling the temperature at 20 ℃ and pH 7; in each stage of extraction process, the stirring time is 30min, and the standing phase separation time is 30 min.
The content of the 1-methylnaphthalene emulsified oil in the wastewater after the extraction treatment is detected to be 40mg/L, and the removal rate of the 1-methylnaphthalene emulsified oil is 97.94%; the content of n-nonanol in the extracted wastewater is less than 100 mg/L.
Example 2
The method treats emulsified oil wastewater with the emulsified oil content of 1383mg/L of 1-methylnaphthalene, and the emulsified oil wastewater and n-nonanol are mixed according to the volume ratio of 3: 1, carrying out secondary cross-flow extraction; extraction conditions are as follows: controlling the temperature at 70 ℃ and pH to 7; in each stage of extraction process, stirring time is 60min, and standing phase separation time is 30 min.
Detecting that the content of the 1-methylnaphthalene emulsified oil in the wastewater after extraction treatment is less than 30mg/L, and the removal rate of the 1-methylnaphthalene emulsified oil is more than 97.83%; the content of n-nonanol in the extracted wastewater is less than 100 mg/L.
Example 3
The emulsified oil wastewater with the emulsified oil content of 1258mg/L of 1-methylnaphthalene treated by the embodiment is prepared by mixing the emulsified oil wastewater and n-nonanol according to the volume ratio of 2: 1, carrying out secondary cross-flow extraction; extraction conditions are as follows: controlling the temperature at 20 ℃ and pH 8; in each stage of extraction process, the stirring time is 30min, and the standing phase separation time is 30 min.
Detecting that the content of the 1-methylnaphthalene emulsified oil in the wastewater after extraction treatment is less than 30mg/L, and the removal rate of the 1-methylnaphthalene emulsified oil is more than 97.61%; the content of n-nonanol in the extracted wastewater is less than 100 mg/L.
Example 4
The emulsified oil wastewater with the emulsified oil content of 1-methylnaphthalene of 760mg/L is treated in the embodiment, and the emulsified oil wastewater and n-nonanol are mixed according to the volume ratio of 7: 1, carrying out secondary cross-flow extraction; extraction conditions are as follows: controlling the temperature at 20 ℃ and pH 8; in each stage of extraction process, the stirring time is 30min, and the standing phase separation time is 30 min.
Detecting that the content of the 1-methylnaphthalene emulsified oil in the wastewater after extraction treatment is less than 30mg/L, and the removal rate of the 1-methylnaphthalene emulsified oil is more than 96.05%; the content of n-nonanol in the extracted wastewater is less than 100 mg/L.
Example 5
The emulsified oil wastewater with the 1-methylnaphthalene emulsified oil content of 1149mg/L is treated by the embodiment, and the emulsified oil wastewater and n-nonanol are mixed according to the volume ratio of 6: 1, carrying out secondary cross-flow extraction; extraction conditions are as follows: controlling the temperature at 20 ℃ and pH to 6; in each stage of extraction process, stirring time is 30min, and standing phase separation time is 60 min.
Detecting that the content of the 1-methylnaphthalene emulsified oil in the wastewater after extraction treatment is less than 30mg/L, and the removal rate of the 1-methylnaphthalene emulsified oil is more than 97.39%; the content of n-nonanol in the extracted wastewater is less than 100 mg/L.
Example 6
The emulsified oil wastewater with 1-methylnaphthalene emulsified oil content of 1089mg/L is treated by the embodiment, and the emulsified oil wastewater and n-nonanol are mixed according to the volume ratio of 6: 1, carrying out secondary cross-flow extraction; extraction conditions are as follows: controlling the temperature at 20 ℃ and pH to 9; in each stage of extraction process, the stirring time is 30min, and the standing phase separation time is 60 min.
Detecting that the content of the 1-methylnaphthalene emulsified oil in the wastewater after extraction treatment is less than 30mg/L, and the removal rate of the 1-methylnaphthalene emulsified oil is more than 97.24%; the content of n-nonanol in the extracted wastewater is less than 100 mg/L.
Example 7
The emulsified oil wastewater with 1-methylnaphthalene emulsified oil content of 1147mg/L is treated by the embodiment, and the emulsified oil wastewater and n-nonanol are mixed according to the volume ratio of 4: 1, carrying out secondary cross-flow extraction; extraction conditions are as follows: controlling the temperature at 20 ℃ and pH 7; in each stage of extraction process, stirring time is 60min, and standing phase separation time is 60 min.
Detecting that the content of the 1-methylnaphthalene emulsified oil in the wastewater after extraction treatment is less than 30mg/L, and the removal rate of the 1-methylnaphthalene emulsified oil is more than 97.38%; the content of n-nonanol in the extracted wastewater is less than 100 mg/L.
Example 8
The emulsified oil wastewater with the emulsified oil content of 976mg/L of 1-methylnaphthalene is treated in the embodiment, and the emulsified oil wastewater and n-nonanol are mixed according to the volume ratio of 5:1, carrying out secondary cross-flow extraction; extraction conditions are as follows: controlling the temperature at 20 ℃ and pH to 9; in each stage of extraction process, the stirring time is 30min, and the standing phase separation time is 30 min.
Detecting that the content of the 1-methylnaphthalene emulsified oil in the wastewater after extraction treatment is less than 30mg/L, and the removal rate of the 1-methylnaphthalene emulsified oil is more than 96.92%; the content of n-nonanol in the extracted wastewater is less than 100 mg/L.
Example 9
The emulsified oil wastewater with the emulsified oil content of 1156mg/L of 1-ethylnaphthalene is treated in the embodiment, and the emulsified oil wastewater and n-nonanol are subjected to secondary cross-flow extraction according to the volume ratio of 5: 1; extraction conditions are as follows: controlling the temperature at 20 ℃ and pH 7; in each stage of extraction process, the stirring time is 30min, and the standing phase separation time is 30 min.
Detecting that the content of the 1-ethylnaphthalene emulsified oil in the wastewater after extraction treatment is less than 30mg/L, and the removal rate of the 1-ethylnaphthalene emulsified oil is more than 97.4%; the content of n-nonanol in the extracted wastewater is less than 100 mg/L.
Example 10
The emulsified oil wastewater with the 2-methylbiphenyl emulsified oil content of 1756mg/L is treated by the embodiment, and the emulsified oil wastewater and n-nonanol are subjected to secondary cross-flow extraction according to the volume ratio of 5: 1; extraction conditions are as follows: controlling the temperature at 20 ℃ and pH 7; in each stage of extraction process, the stirring time is 30min, and the standing phase separation time is 30 min.
The content of the 2-methyl biphenyl emulsified oil in the wastewater after the extraction treatment is detected to be 36mg/L, and the removal rate of the 2-methyl biphenyl emulsified oil is more than 97.9 percent; the content of n-nonanol in the extracted wastewater is less than 100 mg/L.
Example 11
The emulsified oil wastewater with the 2-methyl acenaphthene emulsified oil content of 1364mg/L is treated by the embodiment, and the emulsified oil wastewater and n-nonanol are subjected to secondary cross-flow extraction according to the volume ratio of 5: 1; extraction conditions are as follows: controlling the temperature at 20 ℃ and pH 7; in each stage of extraction process, the stirring time is 30min, and the standing phase separation time is 30 min.
Detecting that the content of the 2-methyl acenaphthene emulsified oil in the wastewater after extraction treatment is less than 30mg/L, and the removal rate of the 2-methyl acenaphthene emulsified oil is more than 97.8%; the content of n-nonanol in the extracted wastewater is less than 100 mg/L.
From the results of the above examples, it can be seen that the method provided by the invention has a significant effect on the extraction of the oil-containing wastewater in the simulated coal chemical industry by using the 1-methylnaphthalene, 1-ethylnaphthalene, 2-methylbiphenyl and 2-methylacenaphthylene emulsified oil. Through two-stage extraction, the content of emulsified oil in simulated wastewater can be less than 50mg/L, and the removal rate of the emulsified oil is more than 96%.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The application of n-nonanol as an extracting agent in separating emulsified oil in coal chemical industry oil-containing wastewater.
2. A method for separating emulsified oil from oily wastewater in coal chemical industry is characterized by comprising the following steps: the method takes n-nonanol as an extracting agent to carry out multi-stage cross-flow extraction on the coal chemical industry oily wastewater, thereby realizing the separation of emulsified oil in the coal chemical industry oily wastewater.
3. The method for separating emulsified oil from oily wastewater in coal chemical industry according to claim 2, wherein the content of emulsified oil in the oily wastewater in coal chemical industry is 500 mg/L-2000 mg/L.
4. The method for separating emulsified oil from coal chemical industry oily wastewater according to claim 2, wherein the volume ratio of the n-nonanol to the coal chemical industry oily wastewater is 1 (2-7).
5. The method for separating emulsified oil from coal chemical industry oily wastewater according to claim 2, wherein the coal chemical industry oily wastewater is semi-coke wastewater.
6. The method for separating emulsified oil from oily wastewater in coal chemical industry according to claim 2, wherein the emulsified oil in oily wastewater in coal chemical industry is emulsified oil containing naphthalene compounds.
7. The method for separating emulsified oil from oily wastewater in coal chemical industry according to claim 2, wherein the multistage cross-flow extraction is performed under the condition that the pH value is 6-12.
8. The method for separating the emulsified oil from the oily wastewater in the coal chemical industry according to claim 2, wherein the multistage cross-flow extraction is performed at a temperature of 20-70 ℃.
9. The method for separating the emulsified oil from the oily wastewater in the coal chemical industry according to claim 2, wherein in the multistage cross-flow extraction process, the stirring time of each stage of extraction is 30-60 min, and the standing phase separation time is 30-60 min.
10. The method for separating the emulsified oil from the oily wastewater in the coal chemical industry according to claim 2, wherein after the multistage cross-flow extraction, a hydrocyclone is adopted to accelerate a part of emulsified oil in the extraction phase to aggregate and separate from the extraction phase.
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