CN113526746A - Method for removing sulfur ions in oil and gas field sewage - Google Patents
Method for removing sulfur ions in oil and gas field sewage Download PDFInfo
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- CN113526746A CN113526746A CN202110979918.5A CN202110979918A CN113526746A CN 113526746 A CN113526746 A CN 113526746A CN 202110979918 A CN202110979918 A CN 202110979918A CN 113526746 A CN113526746 A CN 113526746A
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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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
- C02F2101/10—Inorganic compounds
- C02F2101/101—Sulfur compounds
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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
- C02F2101/40—Organic compounds containing sulfur
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/10—Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/18—Nature of the water, waste water, sewage or sludge to be treated from the purification of gaseous effluents
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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
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention provides a method for removing sulfur ions in oil and gas field sewage, belonging to the technical field of sewage sulfur removal. The invention takes sodium dimethyldithiocarbamate (sodium dimethyl dithiocarbamate) as a desulfurizer, and the sodium dimethyldithiocarbamate contains sulfo-amino which can react with thiadiazine substances to generate water-insoluble substances, thereby removing the thiadiazine organic sulfide; the invention uses soluble trivalent ferric salt and H2O2The solution is used as a precipitation-oxidation system and can remove S in the sewage of the oil and gas field2‑、SH‑And soluble H2And S. Therefore, the temperature of the molten metal is controlled,the method provided by the invention can be used for fully removing sulfur ions in the sulfur-containing wastewater of the oil and gas field, and the results of the embodiment show that the removal rate of sulfur ions in the sewage of the oil and gas field is more than or equal to 85%.
Description
Technical Field
The invention relates to the technical field of sewage desulphurization, in particular to a method for removing sulfur ions in sewage in an oil and gas field.
Background
With the rapid development of the petrochemical industry and the continuous progress of oil and gas exploitation technology, in the exploitation process, a triazine desulfurizer (mainly comprising hydroxyethyl hexahydro-s-triazine) is used by workers to remove hydrogen sulfide gas in natural gas. After the triazine desulfurizer is combined with hydrogen sulfide, a soluble organic sulfide (such as thiadiazine substances) can be formed and dissolved in the oil field sewage, so that the difficulty in removing sulfur ions in the oil field sewage is greatly increased.
At present, the sulfur ions (mainly S ionized from soluble sulfide) in the sewage2-、SH-And soluble H2S) removing methods comprise a chemical precipitation method and a chemical oxidation method, wherein the chemical precipitation method is to utilize a precipitator to react with sulfur ions to generate precipitates so as to achieve the effect of removing the sulfur ions, and the commonly used precipitator is ferric salt, cupric salt and the like; the chemical oxidation method is to oxidize sulfur ions by adopting an oxidant to generate a sulfur simple substance, a high-valence sulfur-containing oxide and the like, thereby realizing the removal of the sulfur ions.
However, since the sulfur-containing pollutant components of the oil and gas field sewage are complex and the difficulty of removing sulfur ions is high, the above method for removing sulfur ions cannot achieve a good removal effect.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for removing sulfur ions from oil and gas field wastewater. The method provided by the invention can effectively remove sulfur ions in the wastewater of the oil and gas field.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for removing sulfur ions in oil and gas field sewage, which comprises the following steps:
(1) stirring and mixing oil-gas field sewage and sodium dimethyldithiocarbamate to obtain a first liquid;
(2) mixing the first liquid with a first flocculating agent, performing first flocculation, and performing solid-liquid separation to obtain a second liquid;
(3) mixing the second liquid with a soluble ferric salt, H2O2Stirring and mixing the solution to obtain a third liquid;
(4) and adjusting the pH value of the third liquid to 7.5-8.5, and adding a second flocculating agent to perform second flocculation.
Preferably, the concentration of the sulfur ions in the oil and gas field sewage in the step (1) is 1000-15000 mg/L.
Preferably, the pH value of the oil-gas field sewage in the step (1) is 6-9.
Preferably, the mass of the sodium dimethyldithiocarbamate in the step (1) is 0.5-1% of the mass of the oil-gas field sewage.
Preferably, the stirring and mixing time in the step (1) is 30-60 min.
Preferably, the first flocculating agent and the second flocculating agent are independently one or more of PAM anionic flocculating agent, PAM cationic flocculating agent and organic amine flocculating agent.
Preferably, the ratio of the mass of the first flocculating agent to the volume of the first liquid in the step (1) is 5-20 mg: 1L of the compound.
Preferably, the soluble ferric salt in the step (3) is one or more of ferric chloride, ferric sulfate and ferric nitrate, and the mass ratio of the soluble ferric salt to the second liquid is (1-3 g): 1L of the compound.
Preferably, H in said step (3)2O2The mass concentration of the solution is 27.5-30%, and the content of H is2O2The mass ratio of the solution to the second liquid is 3-8 g: 1L of the compound.
Preferably, the ratio of the mass of the second flocculating agent to the volume of the third liquid in the step (4) is 5-20 mg: 1L of the compound.
The invention provides a method for removing oil gasThe method for sulfur ions in field sewage comprises the following steps: (1) stirring and mixing oil-gas field sewage and sodium dimethyldithiocarbamate to obtain a first liquid; (2) mixing the first liquid with a first flocculating agent, performing first flocculation, and performing solid-liquid separation to obtain a second liquid; (3) mixing the second liquid with a soluble ferric salt, H2O2Stirring and mixing the solution to obtain a third liquid; (4) and adjusting the pH value of the third liquid to 7.5-8.5, and adding a second flocculating agent to perform second flocculation. The invention takes sodium dimethyldithiocarbamate (sodium dimethyl dithiocarbamate) as a desulfurizer, and the sodium dimethyldithiocarbamate contains sulfo-amino which can react with thiadiazine substances to generate water-insoluble substances, thereby removing the thiadiazine organic sulfide; the invention uses soluble trivalent ferric salt and H2O2The solution is used as a precipitation-oxidation system and can remove S in the sewage of the oil and gas field2-、SH-And soluble H2And S. Therefore, the method provided by the invention can sufficiently remove the sulfur ions in the sulfur-containing wastewater of the oil and gas field, and the example results show that when the concentration of the sulfur ions in the raw water is 8000mg/L, the content of the sulfur ions after sulfur removal by long time is 856mg/L, and the removal rate of the sulfur ions is more than or equal to 85%.
Detailed Description
The invention provides a method for removing sulfur ions in oil and gas field sewage, which comprises the following steps:
(1) stirring and mixing oil-gas field sewage and sodium dimethyldithiocarbamate to obtain a first liquid;
(2) mixing the first liquid with a first flocculating agent, performing first flocculation, and performing solid-liquid separation to obtain a second liquid;
(3) mixing the second liquid with a soluble ferric salt, H2O2Stirring and mixing the solution to obtain a third liquid;
(4) and adjusting the pH value of the third liquid to 7.5-8.5, and adding a second flocculating agent to perform second flocculation.
The invention mixes the oil-gas field sewage and the dimethyl sodium dithiocarbamate to obtain the first liquid. The method has no special requirements on the type and source of the oil-gas field sewage, and the oil-gas field sewage known in the field can remove the sulfur ions by using the method provided by the invention. In the present invention, the oil and gas field wastewater preferably contains a thiadiazine-type soluble organic sulfide.
In the invention, the sulfur ion concentration of the oil-gas field sewage is preferably 1000-15000 mg/L, and more preferably 5000-8000 mg/L.
In the invention, the pH value of the oil-gas field sewage is preferably 6-9, and more preferably 6-8. In the invention, when the pH value of the oil and gas field sewage does not meet the requirement, the pH value of the oil and gas field sewage is preferably adjusted; the present invention does not require any particular kind of agent for adjusting pH, and a pH adjuster known to those skilled in the art may be used.
In the invention, the mass of the sodium dimethyldithiocarbamate is preferably 0.5-1% of the mass of the sulfur-containing sewage, and more preferably 0.6-0.8%. The invention has no special requirement on the source of the sodium dimethyldithiocarbamate (sodium ferbamate), and the sodium dimethyldithiocarbamate which is conventional and commercially available in the field can be used. As an embodiment of the present invention, the sodium dimethyldithiocarbamate is available from Shigan chemical company.
In the invention, the time for stirring and mixing the oil-gas field sewage and the sodium dimethyldithiocarbamate is preferably 30-60 min, and more preferably 40-50 min. The invention has no special requirement on the stirring speed, and can ensure that the sewage of the oil-gas field and the sodium dimethyldithiocarbamate are fully mixed.
After the first liquid is obtained, the first liquid and a first flocculating agent are mixed for first flocculation, and a second liquid is obtained after solid-liquid separation. In the invention, the first flocculating agent is preferably one or more of PAM anionic flocculating agent, PAM cationic flocculating agent and organic amine flocculating agent; in the invention, the molecular weight of the PAM anionic flocculant is preferably 800-1200 ten thousand, and more preferably 900-1000 ten thousand; the ion degree of the PAM cationic flocculant is preferably 45-80%, and more preferably 60-70%; the content of effective components in the organic amine type flocculating agent is 40-60%, and more preferably 50%. The PAM anionic flocculant has no special requirement on the source, and the PAM anionic flocculant which is conventionally sold in the field can be used; as a specific example of the present invention, the PAM anionic flocculant is purchased from the institute of chemical engineering, Zhonghai oil Tianjin.
According to the invention, the first flocculation is preferably carried out under a standing condition, and the time of the first flocculation is preferably 2-10 min, and more preferably 3-5 min. In the invention, the ratio of the mass of the first flocculating agent to the volume of the first liquid is preferably 5-20 mg: 1L, more preferably 10-15 mg: 1L of the compound.
The present invention has no special requirement on the solid-liquid separation mode, and the solid-liquid separation mode known to those skilled in the art can be used, such as filtration.
After the second liquid is obtained, the invention mixes the second liquid with soluble ferric salt and H2O2The solution is stirred and mixed to obtain a third liquid. In the invention, the soluble ferric salt is preferably one or more of ferric chloride, ferric sulfate and ferric nitrate, and the mass ratio of the soluble ferric salt to the second liquid is preferably 1-3 g: 1L, more preferably 2 g: 1L of the compound.
In the present invention, said H2O2The mass concentration of the solution is preferably 27.5-30%, and more preferably 28-29%; said H2O2The mass ratio of the solution to the volume of the second liquid is preferably 3-8 g: 1L, more preferably 4-6 g: 1L of the compound.
In the present invention, the mixing is preferably performed in the following manner:
mixing the second liquid with soluble ferric salt, and carrying out first stirring; adding H into the obtained mixed solution2O2And (4) carrying out second stirring on the solution.
In the invention, the first stirring speed is preferably 100-300 r/min, more preferably 150-200 r/min, and the time is preferably 30-90 min, more preferably 50-80 min; the second stirring speed is preferably 100-300 r/min, more preferably 150-200 r/min, and the time is preferably 30-90 min, more preferably 50-80 min.
After the third liquid is obtained, the pH value of the third liquid is adjusted to 7.5-8.5, and a second flocculating agent is added for second flocculation. In the invention, the pH value adjusting reagent is preferably a sodium hydroxide solution, and the mass concentration of the sodium hydroxide solution is preferably 5-40%, and more preferably 15-25%. In the invention, the second flocculating agent is preferably one or more of PAM anionic flocculating agent, PAM cationic flocculating agent and organic amine flocculating agent; in the invention, the molecular weight of the PAM anionic flocculant is preferably 800-1200 ten thousand, and more preferably 900-1000 ten thousand; the ion degree of the PAM cationic flocculant is preferably 45-80%, and more preferably 60-70%; the content of effective components in the organic amine type flocculating agent is 40-60%, and more preferably 50%. The PAM anionic flocculant has no special requirement on the source, and the PAM anionic flocculant which is conventionally sold in the field can be used; as a specific example of the present invention, the PAM anionic flocculant is purchased from the institute of chemical engineering, Zhonghai oil Tianjin.
According to the invention, the second flocculation is preferably carried out under a standing condition, and the time of the second flocculation is preferably 2-10 min, and more preferably 3-5 min. In the invention, the ratio of the mass of the second flocculating agent to the volume of the second liquid is preferably 5-20 mg: 1L, more preferably 10-15 mg: 1L of the compound.
After the second flocculation, solid-liquid separation is preferably carried out in the invention to obtain the oil-gas field sewage from which the sulfur ions are removed. The present invention has no special requirement on the solid-liquid separation mode, and the solid-liquid separation mode known to those skilled in the art can be used, such as filtration.
The method for removing sulfur ions from oil and gas field wastewater according to the present invention will be described in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention.
In the following examples, the detection method of the sulfide ion concentration is as follows: GB/T16489-1996 hydrosulfide determination methylene blue spectrophotometry.
Example 1
Taking oil and gas field sewage, wherein the concentration of sulfur ions in raw water is 8000mg/L, the pH value is 6, directly adding sodium dimethyl sulfate solid with the mass of 0.5 percent of the sewage into the water, stirring for 30 minutes, adding 15mg/L PAM anions with the molecular weight of 800 ten thousand for flocculation, standing and settling, taking the supernatant after settling, adding 2000mg/L ferric chloride, stirring and reacting for 60 minutes, adding 7000mg/L hydrogen peroxide with the concentration of 27.5wt percent, stirring for 60 minutes, adding a sodium hydroxide solution, adjusting the pH value to 8.5, adding 15mg/L PAM anions with the molecular weight of 800 ten thousand for flocculation, standing and settling, taking the supernatant to detect the concentration of sulfur ions, and detecting the concentration of sulfur ions to be 3210 mg/L.
Example 2
Taking oil and gas field sewage, wherein the concentration of sulfur ions in raw water is 8000mg/L, the pH is 6, using a sodium hydroxide solution with the concentration of 10 wt%, adjusting the pH of the waste water to 7, adding sodium ferulate solid with the mass of 0.5% of the sewage into the water, stirring for 30 minutes, adding PAM anions with the molecular weight of 15mg/L and the molecular weight of 1000 ten thousand for flocculation, standing for sedimentation, taking the supernatant after sedimentation, adding iron chloride with the molecular weight of 2000mg/L, stirring for reaction for 60 minutes, adding hydrogen peroxide with the concentration of 7000mg/L and the concentration of 27.5 wt%, stirring for 60 minutes, adding a sodium hydroxide solution, adjusting the pH to 8.5, adding PAM anions with the molecular weight of 15mg/L and the molecular weight of 1000 ten thousand for flocculation, standing for sedimentation, taking the supernatant, detecting the concentration of sulfur ions, and obtaining the concentration of the treated sulfur ions to be 4523 mg/L.
Example 3
Taking oil and gas field sewage, wherein the concentration of sulfur ions in raw water is 8000mg/L, the pH is 6, using a sodium hydroxide solution with the concentration of 10 wt%, adjusting the pH of the waste water to 8, adding sodium ferulate solid with the mass of 0.5% of the sewage into the water, stirring for 30 minutes, adding PAM anions with the molecular weight of 15mg/L and 1200 ten thousand for flocculation, standing for sedimentation, taking the supernatant after sedimentation, adding iron chloride with the molecular weight of 2000mg/L, stirring for reaction for 60 minutes, adding hydrogen peroxide with the concentration of 7000mg/L and the concentration of 27.5 wt%, stirring for 60 minutes, adding a sodium hydroxide solution, adjusting the pH to 8.5, adding PAM anions with the molecular weight of 15mg/L and 1200 ten thousand for flocculation, standing for sedimentation, taking the supernatant, detecting the concentration of sulfur ions, and obtaining the concentration of the treated sulfur ions to be 4956 mg/L.
Example 4
Taking oil and gas field sewage, wherein the concentration of sulfur ions in raw water is 8000mg/L, the pH value is 6, directly adding sodium dimethyl sulfate solid with the mass of 1% of the sewage into the water, stirring for 30 minutes, adding 15mg/L PAM anions with the molecular weight of 800 ten thousand for flocculation, standing and settling, taking supernatant after settling, adding 2000mg/L ferric chloride, stirring and reacting for 60 minutes, adding 7000mg/L hydrogen peroxide with the concentration of 27.5 wt%, stirring for 60 minutes, adding a sodium hydroxide solution, adjusting the pH value to 8.5, adding 15mg/L PAM anions with the molecular weight of 800 ten thousand for flocculation, standing and settling, taking supernatant, detecting the concentration of sulfur ions, and obtaining the treated concentration of sulfur ions of 856 mg/L.
Example 5
Taking oil and gas field sewage, wherein the concentration of sulfur ions in raw water is 8000mg/L, the pH is 6, using a sodium hydroxide solution with the concentration of 10 wt%, adjusting the pH of the waste water to 7, adding thiram solid with the mass of 1% of the sewage into the water, stirring for 30 minutes, adding 15mg/L PAM anions for flocculation, standing for sedimentation, taking a supernatant after sedimentation, adding 2000mg/L ferric chloride, stirring for reaction for 60 minutes, adding 7000mg/L hydrogen peroxide with the concentration of 27.5 wt%, stirring for 60 minutes, adding the sodium hydroxide solution, adjusting the pH to 8.5, adding 15mg/L PAM anions for flocculation, standing for sedimentation, taking the supernatant, detecting the concentration of the sulfur ions, and detecting the concentration of the sulfur ions after treatment to be 2891 mg/L.
Example 6
Taking oil and gas field sewage, wherein the concentration of sulfur ions in raw water is 8000mg/L, the pH is 6, using a sodium hydroxide solution with the concentration of 10 wt%, adjusting the pH of the waste water to 8, adding sodium ferulate solid with the mass of 1% of the sewage into the water, stirring for 30 minutes, adding PAM anions with the molecular weight of 15mg/L and the molecular weight of 800 ten thousand for flocculation, standing for sedimentation, taking the supernatant after sedimentation, adding iron chloride with the molecular weight of 2000mg/L, stirring for reaction for 60 minutes, adding hydrogen peroxide with the concentration of 7000mg/L and the concentration of 27.5 wt%, stirring for 60 minutes, adding a sodium hydroxide solution, adjusting the pH to 8.5, adding PAM anions with the molecular weight of 15mg/L and the molecular weight of 800 ten thousand for flocculation, standing for sedimentation, taking the supernatant, detecting the concentration of sulfur ions, and detecting the concentration of the sulfur ions after treatment to be 3452 mg/L.
Comparative example 1
Taking oil and gas field sewage, wherein the concentration of sulfur ions in raw water is 8000mg/L, the pH value is 6, directly adding 2000mg/L ferric chloride into the water, stirring and reacting for 60 minutes, then adding 7000mg/L hydrogen peroxide with the concentration of 27.5 wt%, stirring for 60 minutes, adding sodium hydroxide solution, adjusting the pH value to 8.5, adding 15mg/L PAM anion with the molecular weight of 800 ten thousand for flocculation, standing and settling, taking supernatant, detecting the concentration of the sulfur ions, and obtaining the concentration of the processed sulfur ions which is 6891 mg/L.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for removing sulfur ions in sewage of an oil and gas field comprises the following steps:
(1) stirring and mixing oil-gas field sewage and sodium dimethyldithiocarbamate to obtain a first liquid;
(2) mixing the first liquid with a first flocculating agent, performing first flocculation, and performing solid-liquid separation to obtain a second liquid;
(3) mixing the second liquid with a soluble ferric salt, H2O2Stirring and mixing the solution to obtain a third liquid;
(4) and adjusting the pH value of the third liquid to 7.5-8.5, and adding a second flocculating agent to perform second flocculation.
2. The method according to claim 1, wherein the oil and gas field wastewater in the step (1) has a sulfur ion concentration of 1000 to 15000 mg/L.
3. The method according to claim 1, wherein the pH of the oil and gas field wastewater in the step (1) is 6 to 9.
4. The method according to claim 1 or 2, wherein the mass of the sodium dimethyldithiocarbamate in the step (1) is 0.5-1% of the mass of the oil and gas field sewage.
5. The method according to claim 1, wherein the stirring and mixing time in the step (1) is 30-60 min.
6. The method of claim 1, wherein the first and second flocculants are independently one or more of a PAM anionic flocculant, a PAM cationic flocculant, and an organic amine flocculant.
7. The method according to claim 1 or 6, wherein the ratio of the mass of the first flocculating agent to the volume of the first liquid in step (1) is 5-20 mg: 1L of the compound.
8. The method according to claim 1, wherein the soluble ferric salt in the step (3) is one or more of ferric chloride, ferric sulfate and ferric nitrate, and the mass ratio of the soluble ferric salt to the second liquid is 1-3 g: 1L of the compound.
9. The method of claim 1, wherein H in step (3)2O2The mass concentration of the solution is 27.5-30%, and the content of H is2O2The mass ratio of the solution to the second liquid is 3-8 g: 1L of the compound.
10. The method according to claim 1 or 6, wherein the ratio of the mass of the second flocculating agent to the volume of the third liquid in the step (4) is 5-20 mg: 1L of the compound.
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| CN117658395A (en) * | 2024-02-02 | 2024-03-08 | 克拉玛依市三达新技术股份有限公司 | Treatment method of wastewater containing hydrogen sulfide |
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| CN110980863A (en) * | 2019-12-24 | 2020-04-10 | 苏州科镭沃环保科技有限公司 | Desulfurization wastewater comprehensive treatment agent and preparation method thereof |
Cited By (1)
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| CN117658395A (en) * | 2024-02-02 | 2024-03-08 | 克拉玛依市三达新技术股份有限公司 | Treatment method of wastewater containing hydrogen sulfide |
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