CN113003826A - Harmless treatment method of desulfurization waste alkali liquor - Google Patents
Harmless treatment method of desulfurization waste alkali liquor Download PDFInfo
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- CN113003826A CN113003826A CN202110227620.9A CN202110227620A CN113003826A CN 113003826 A CN113003826 A CN 113003826A CN 202110227620 A CN202110227620 A CN 202110227620A CN 113003826 A CN113003826 A CN 113003826A
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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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
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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
- C02F2001/007—Processes including a sedimentation step
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
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- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a harmless treatment method of desulfurization waste alkali liquor, which comprises the following steps of firstly, adsorbing, namely collecting the waste alkali liquor into a gravity sedimentation tank through a liquid discharge pump, adsorbing harmful substances in the waste alkali liquor through a curing base material in the gravity sedimentation tank to form colloid, wherein the curing base material is a mixture of lime or cement kiln dust, diatomite and graphene oxide; and step two, curing and oxidizing, namely pumping the pre-clarified waste alkali liquor into a reaction kettle through a delivery pump, adding quantitative quick lime, stirring, introducing into a rake dryer, drying under the conditions of heating and vacuumizing to form powder, and temporarily storing the powder in a rain-proof shed for natural oxidation and thick handing over to a solid waste treatment unit for subsequent treatment. The harmless treatment method of the desulfurization waste alkali liquor is simple and easy to implement, environment-friendly and low in treatment cost.
Description
The technical field is as follows:
the invention relates to the technical field of petroleum refining, in particular to a harmless treatment method of desulfurization waste alkali liquor.
Background art:
in the process of petroleum refining, desulfurization waste alkali liquor (also called waste alkali liquor and caustic sludge) is one of important pollutants of refining enterprises, the process of removing hydrogen sulfide by using methyldiethanolamine series solution is widely applied at present, and sulfur-containing waste gas released in amine liquid regeneration is preferably prepared into sulfur or sulfuric acid by a Claus process. Limited by the small size of some enterprises and the low sulfur content of raw oil, the sulfur-containing tail gas generated by the enterprises has low sulfur and low flow rate, and can not support the lowest load of the Claus process at all. On the other hand, the sulfur-containing tail gas discharged by the non-hydrogenation device also contains trace phenols and alcohol sulfides, and the wet oxidation process adopting the complex iron solution is also limited. Therefore, the adoption of the sodium hydroxide solution for alkali washing and desulfurization is still a forced choice for realizing standard discharge and clean production of the devices.
The sodium hydroxide solution has extremely strong alkalinity, and can absorb all sulfides, alcohols and phenols in the sulfur-containing noncondensable gas of the non-hydrogenation device and the sulfur-containing sewage stripping gas to form waste alkali liquor (liquid caustic sludge). The alkali liquor has high concentration, high salinity, stink and difficult degradation, is an industrial waste which causes headaches of refining enterprises, wherein a large amount of toxic and harmful substances such as COD, sulfide, volatile phenol and the like seriously pollute the environment, and the existing sewage treatment plants are difficult to treat and easily cause overstocking.
At present, alkali liquor treatment processes which are widely applied can be divided into two major categories, namely an incineration method and a wet oxidation method. The burning method is to burn the alkali liquor by fuel, the sulfide is burnt into sulfur dioxide and phenol alcohol to burn into carbon dioxide and water, and the slaked lime solution is used to absorb the tail gas to realize the solidification and the discharge after reaching the standard. Obviously, the incineration method needs to be provided with a high-temperature corrosion-resistant boiler and a tail gas absorption tower, and needs to supply a large amount of fuel to gasify and fully combust the alkali liquor, so that the investment and the energy consumption are both large.
The wet oxidation process is to pressurize and convey waste alkali liquid, air and steam into an oxidation reactor, after reaction time of more than 40 minutes at 150 ℃ and under 130 ℃, oxygen in the air oxidizes sulfides such as sodium hydrosulfide, sodium mercaptide and the like into more stable salts such as sodium sulfate, sodium thiosulfate and the like, remove odor smell and reduce volatile matters, COD and the like, and the aim of wet oxidation is to convert sodium sulfide into sodium sulfate as much as possible. A large-scale ethylene cracking device is generally required to be provided with a set of alkali liquor treatment device. The treatment device needs to be provided with a storage tank, an oil removal unit, an air compressor unit, a reaction unit, a neutralization unit, a heat exchange and tail gas treatment unit and the like. The wet oxidation method is suitable for enterprises continuously treating a large amount of waste alkali liquor, but has high cost and complex process, and is not suitable for small and medium-sized enterprises.
The invention content is as follows:
the invention aims to solve the technical problem of providing a simple and feasible harmless treatment method of the desulfurization waste alkali liquor, and the harmless treatment method is environment-friendly and has lower treatment cost.
The technical proposal of the invention is to provide a harmless treatment method of the desulfurization waste lye, which comprises the following steps,
absorbing, namely collecting waste alkali liquor into a gravity settling tank through a liquid discharge pump, and absorbing harmful substances in the waste alkali liquor through a curing base material in the gravity settling tank to form a colloid, wherein the curing base material is a mixture of lime or cement kiln dust, diatomite and graphene oxide;
and step two, curing and oxidizing, namely pumping the pre-clarified waste alkali liquor into a reaction kettle through a delivery pump, adding quantitative quick lime, stirring, introducing into a rake dryer, drying under the conditions of heating and vacuumizing to form powder, and temporarily storing the powder in a rain-proof shed for natural oxidation and thick handing over to a solid waste treatment unit for subsequent treatment.
Preferably, the mass ratio of the lime or cement kiln dust to the mixture of the diatomite and the graphene oxide is 3:2: 1.
Preferably, the second step can be replaced by the following operation that the pre-clarified waste alkali liquor in the collecting tank is pumped into an evaporation pond through a delivery pump, the required amount of raw lime is calculated through a titration experiment before the waste alkali liquor is introduced into the evaporation pond, the quick lime is placed into the evaporation pond and then the waste alkali liquor is introduced, so that the volatilization of malodorous components in the waste alkali liquor can be reduced, white powder is formed after stirring, sedimentation, natural oxidation, drying and crushing, and the solid waste treatment unit can be bagged and delivered after weighing without reduction.
Preferably, in the first step, 80% -90% of the waste alkali liquor separated by the combination of gravity settling, vortex separation and coalescence separation after adsorption enters a reaction kettle or an evaporation pond through a delivery pump, and the rest 10% -20% is discharged; burning 10-20% of discharged waste lye in an incinerator, recovering the sodium sulfate part generated after burning, introducing the molten sodium sulfate into a flue together with flue gas when the molten sodium sulfate flows out from the bottom of an incinerator chamber, and recovering the molten sodium sulfate through electrostatic adsorption.
Furthermore, the diatomite is subjected to acid leaching treatment by using diluted sulfuric acid in advance, iron and aluminum impurities in the diatomite are separated, organic matters in inner holes of the diatomite are decomposed, the inner surface area is increased, and the adsorption performance of the diatomite is improved. The adsorption effect is improved.
Compared with the prior art, the invention has the following advantages after adopting the scheme: harmful substances in the waste alkali liquor are adsorbed by a solidified base material in the gravity sedimentation tank to form colloid, the waste alkali liquor and the quick lime are mixed, solidified and naturally oxidized, the volume of the waste alkali liquor can be concentrated to one third of the original volume, and the transportation cost of industrial wastes is reduced; lime solidification reduces the harm of alkali liquor, promotes sulfide to be oxidized into sulfate, the treatment method is simple and easy to implement, and can effectively reduce the treatment cost.
The specific implementation mode is as follows:
the invention is further illustrated with respect to specific embodiments below:
example one
A harmless treatment method of desulfurization waste lye, which comprises the following steps,
the method comprises the following steps of firstly, adsorbing, namely collecting waste alkali liquor into a gravity sedimentation tank through a liquid discharge pump, adsorbing harmful substances in the waste alkali liquor through a solidification substrate positioned in the gravity sedimentation tank to form colloid, wherein the solidification substrate is a mixture of lime or cement kiln dust, diatomite and graphene oxide, preferably, the mixture of the lime or cement kiln dust, the diatomite and the graphene oxide is in a mass ratio of 3:2:1, and the diatomite is subjected to acid leaching treatment by using diluted sulfuric acid in advance to separate iron and aluminum impurities in the diatomite and decompose organic matters in inner holes of the diatomite at the same time, so that the inner surface area is increased, and the adsorption performance of the diatomite is improved. The adsorption effect is improved;
and step two, curing and oxidizing, namely pumping the pre-clarified waste alkali liquor into a reaction kettle through a delivery pump, adding quantitative quick lime, stirring, introducing into a rake dryer, drying under the conditions of heating and vacuumizing to form powder, and temporarily storing the powder in a rain-proof shed for natural oxidation and thick handing over to a solid waste treatment unit for subsequent treatment.
The embodiment is suitable for enterprises in humid areas, considering that the evaporation pond is likely to be difficult to realize evaporation weight reduction, titration analysis is not performed firstly, the lime amount to be mixed is determined, then the lime is mixed and stirred with the alkali liquor to be treated, the mixture is introduced into a rake dryer, the mixture is dried under the conditions of heating and vacuumizing to form powder, the powder is temporarily stored in a rain-proof shed for natural oxidation, the COD of the powder solution is periodically analyzed, and the oxidation degree is judged. Or the powder is directly delivered to a solid waste treatment unit without temporary storage, and the method is also feasible.
After the waste alkali liquor is neutralized by lime and naturally oxidized for a period of time, most of sulfides, mercaptan and the like in the waste alkali liquor can be oxidized into sulfates and solidified, and the generated solid salts (calcium sulfate, sodium sulfate and the like) belong to low-toxicity industrial wastes and can be handed to a solid waste treatment company for landfill after being treated by a standard procedure.
The method for treating the waste alkali liquor by using quicklime curing and natural oxidation can concentrate the volume of the waste alkali liquor to one third of the original volume, thereby reducing the transportation cost of industrial waste; lime solidification reduces the harm of alkali liquor, promotes sulfide to be oxidized into sulfate, avoids possible leakage risk in the process of transporting waste alkali liquor, and belongs to a simpler, more convenient and more economic waste treatment process. Although the solid waste disposal unit still needs to be handed over, the total amount is reduced, the hazard is reduced, and the solid waste disposal unit is also beneficial to be disposed separately. The colloid formed by adsorption can be treated by a solid waste treatment unit after being dried.
Example 2
A harmless treatment method of desulfurization waste lye, which comprises the following steps,
the method comprises the following steps of firstly, adsorbing, namely collecting waste alkali liquor into a gravity sedimentation tank through a liquid discharge pump, adsorbing harmful substances in the waste alkali liquor through a solidification substrate positioned in the gravity sedimentation tank to form colloid, wherein the solidification substrate is a mixture of lime or cement kiln dust, diatomite and graphene oxide, preferably, the mixture of the lime or cement kiln dust, the diatomite and the graphene oxide is in a mass ratio of 3:2:1, and the diatomite is subjected to acid leaching treatment by using diluted sulfuric acid in advance to separate iron and aluminum impurities in the diatomite and decompose organic matters in inner holes of the diatomite at the same time, so that the inner surface area is increased, and the adsorption performance of the diatomite is improved. The adsorption effect is improved;
step two, pumping the pre-clarified waste alkali liquor in the collecting tank into an evaporation pond through a delivery pump, calculating the required lime amount through a titration experiment before introducing the waste alkali liquor into the evaporation pond, firstly placing quicklime into the evaporation pond, then introducing the waste alkali liquor, reducing the volatilization of offensive odor components in the waste alkali liquor, forming white powder after stirring, settling, natural oxidation, drying and crushing, bagging and delivering the white powder to a solid waste treatment unit when no reduction is caused by weighing
The treatment method of the embodiment is suitable for small and medium-sized enterprises which are located in arid areas and generate hundreds of thousands of tons of waste alkali liquor annually, and an anti-leakage evaporation pond is not constructed according to the standard requirement. The depth of the evaporation pond is not suitable to exceed the local net evaporation capacity, the width of the evaporation pond is suitable to facilitate manual cleaning of two sides, and the area of the evaporation pond is determined by combining the waste alkali liquor of the enterprise and the reserved industrial land. Considering that the wind power can blow off the powder, the evaporation pond needs to consider a covering measure to avoid the flying of the powder.
In addition, in order to carry out treatment more effectively, in the step one, 80% -90% of waste alkali liquor separated by the combination of gravity settling, vortex separation and coalescence separation enters a reaction kettle or an evaporation pond through a delivery pump, and the rest 10% -20% of waste alkali liquor is discharged (the part is mainly the waste alkali liquor on the uppermost surface of the gravity settling tank); burning 10-20% of discharged waste lye in an incinerator, recovering the sodium sulfate part generated after burning, introducing the molten sodium sulfate into a flue together with flue gas when the molten sodium sulfate flows out from the bottom of an incinerator chamber, and recovering the molten sodium sulfate through electrostatic adsorption.
For proving effectiveness, adding 15g of quicklime into 100ml of yellow-green waste alkali liquor in the step one, and stirring to form light blue viscous colloid; after standing for 2 hours, no precipitate and clear liquid were formed. The laboratory staff firstly detects through the four-in-one detector, finds that volatile components in the laboratory beaker can not be detected, and the smell of the volatile components is close to the sludge at the bottom of the water treatment tank. And placing the ash-added slurry and the stock solution sample in outdoor sunlight for natural oxidation. After three days, the light blue slurry was dried to a dark blue solid; crushing, airing for seven days to obtain light blue powder, and weighing; after ten days, the powder was completely white and the weight was not reduced. The experimenter adds water to the powder again and stirs the powder to the initial liquid level, and stands the powder to form a transparent solution of a small amount of insoluble solids.
And (3) carrying out COD detection on the transparent liquid, adding concentrated sulfuric acid to obtain flocculation precipitation which is a gypsum component, standing for 2 hours, and then measuring supernatant liquid, wherein the result is 5450mg/l, and the COD value is still high and is reduced by nine times compared with the original waste alkali liquor. The pH of the clear solution was also measured separately and showed 11.7, which is close to that of saturated limewater, and it is considered that the amount of lime added was somewhat excessive and that a slight excess of lime was beneficial to stabilize the sulfides and avoid escaping.
The solids after removal of the clear liquid were again air-dried and weighed until no further weight loss, resulting in a solids retention of 67.1%. The main component of the original solid is insoluble calcium sulfate, and the second is soluble sodium sulfate and the like.
The invention has the following advantages: harmful substances in the waste alkali liquor are adsorbed by a solidified base material in the gravity sedimentation tank to form colloid, the waste alkali liquor and the quick lime are mixed, solidified and naturally oxidized, the volume of the waste alkali liquor can be concentrated to one third of the original volume, and the transportation cost of industrial wastes is reduced; lime solidification reduces the harm of alkali liquor, promotes sulfide to be oxidized into sulfate, the treatment method is simple and easy to implement, and can effectively reduce the treatment cost.
The foregoing is illustrative of the preferred embodiments of the present invention only and is not to be construed as limiting the claims. All the equivalent structures or equivalent process changes made by the description of the invention are included in the scope of the patent protection of the invention.
Claims (5)
1. A harmless treatment method of desulfurization waste lye is characterized in that: comprises the following steps of (a) carrying out,
absorbing, namely collecting waste alkali liquor into a gravity settling tank through a liquid discharge pump, and absorbing harmful substances in the waste alkali liquor through a curing base material in the gravity settling tank to form a colloid, wherein the curing base material is a mixture of lime or cement kiln dust, diatomite and graphene oxide;
and step two, curing and oxidizing, namely pumping the pre-clarified waste alkali liquor into a reaction kettle through a delivery pump, adding quantitative quick lime, stirring, introducing into a rake dryer, drying under the conditions of heating and vacuumizing to form powder, and temporarily storing the powder in a rain-proof shed for natural oxidation and thick handing over to a solid waste treatment unit for subsequent treatment.
2. The method for harmless treatment of desulfurization waste lye of claim 1, characterized in that: the mass ratio of the lime or cement kiln dust to the mixture of the diatomite and the graphene oxide is 3:2: 1.
3. The method for harmless treatment of desulfurization waste lye of claim 1, characterized in that: and step two can be replaced by the following operation, the pre-clarified waste alkali liquor in the collecting tank is pumped into an evaporation pond through a conveying pump, the required amount of raw lime is calculated through a titration experiment before the waste alkali liquor is introduced into the evaporation pond, the quick lime is firstly placed into the evaporation pond, then the waste alkali liquor is introduced, the volatilization of malodorous components in the waste alkali liquor can be reduced, white powder is formed after stirring, sedimentation, natural oxidation, drying and crushing, and the solid waste treatment unit can be bagged and delivered after weighing without reduction.
4. The method for harmless treatment of desulfurization waste lye of claim 1, characterized in that: in the first step, 80-90% of the waste alkali liquor separated by the combination of gravity settling, vortex separation and coalescence separation after adsorption enters a reaction kettle or an evaporation pond through a delivery pump, and the rest 10-20% is discharged; burning 10-20% of discharged waste lye in an incinerator, recovering the sodium sulfate part generated after burning, introducing the molten sodium sulfate into a flue together with flue gas when the molten sodium sulfate flows out from the bottom of an incinerator chamber, and recovering the molten sodium sulfate through electrostatic adsorption.
5. The method for harmless treatment of desulfurization waste lye of claim 1 or 2, characterized in that: the diatomite is subjected to acid leaching treatment by using diluted sulfuric acid in advance, iron and aluminum impurities in the diatomite are separated, organic matters in inner holes of the diatomite are decomposed, the inner surface area is increased, and the adsorption performance of the diatomite is improved.
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