CN114249454A - Cleaning method for slime water - Google Patents
Cleaning method for slime water Download PDFInfo
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- CN114249454A CN114249454A CN202111471063.1A CN202111471063A CN114249454A CN 114249454 A CN114249454 A CN 114249454A CN 202111471063 A CN202111471063 A CN 202111471063A CN 114249454 A CN114249454 A CN 114249454A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000004140 cleaning Methods 0.000 title claims abstract description 32
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 77
- 239000003245 coal Substances 0.000 claims abstract description 74
- 230000004913 activation Effects 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000002893 slag Substances 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 9
- 230000003213 activating effect Effects 0.000 claims description 10
- 239000010802 sludge Substances 0.000 claims description 8
- 239000006228 supernatant Substances 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 239000003250 coal slurry Substances 0.000 claims description 6
- 239000004576 sand Substances 0.000 claims description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 14
- 239000011707 mineral Substances 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 10
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- 238000007865 diluting Methods 0.000 description 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000009412 basement excavation Methods 0.000 description 1
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- 231100001234 toxic pollutant Toxicity 0.000 description 1
Images
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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
-
- 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
-
- 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
-
- 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
Abstract
The invention discloses a cleaning method of slime water, which comprises the steps of firstly, carrying out activation treatment on crushed and ground coal gangue under the condition of supercritical or subcritical water so as to reduce the chemical stability of minerals, and carrying out crystal form transformation so as to convert the crushed and ground coal gangue into an amorphous state so as to improve the activity; separating an organic liquid phase and a solid slag phase by strong centrifugal force of a hydrocyclone to realize primary separation of minerals; mixing the organic liquid phase and the hydrogen peroxide solution, reacting for 30-90 min in a supercritical environment at 220-300 ℃ and 15-40 MPa, and cooling and standing the obtained mixed solution to enable the coal slime to quickly sink to the bottom. The invention adopts supercritical treatment after adding hydrogen peroxide to achieve the purpose of quickly treating the slime water, and the method has simple operation, does not consume a large amount of medicines, does not need any catalyst, is not influenced by the water quality, and has better water quality after treatment.
Description
Technical Field
The invention relates to the technical field of slime water treatment, in particular to a method for cleaning slime water.
Background
The coal gangue is a solid waste generated in the production and processing processes of coal, is a coal symbiotic resource, and the production amount of the coal gangue accounts for 10-25% of the coal exploitation amount. The coal gangue comprises gangue discharged during roadway excavation of a coal mine, gangue stripped during open-pit coal mining and gangue discharged during separation processing, and is a mixture consisting of various ore rocks. The coal gangue yield in China is accumulated to exceed 50 hundred million t, the coal gangue utilization rate is only 70 percent, and the utilization rate of developed countries represented by British and America reaches 90 percent. The method shows that the comprehensive utilization degree of the coal gangue is insufficient, the stacking amount is increased day by day, and the environmental problems are increased.
A large amount of coal slime water is generated when coal gangue is treated, and how to treat the generated coal slime water becomes a problem. At present, the traditional treatment processes of the coal slime sewage, such as coagulation, flocculation and the like, have complex operation, are greatly influenced by the quality of the incoming water, consume a large amount of chemicals, have low cleanliness of the treated water, and cannot be used in places with higher water quality requirements, such as domestic water and the like.
Disclosure of Invention
The invention provides a method for cleaning slime water, which is used for overcoming the defects that the prior art is complex in operation, is greatly influenced by the quality of incoming water, consumes a large amount of chemicals, is not high in the cleanliness of the treated water, cannot be used in places with higher water quality requirements such as domestic water and the like.
In order to achieve the purpose, the invention provides a method for cleaning slime water, which comprises the following steps:
s1: performing activation treatment on the crushed and ground coal gangue under the subcritical or supercritical water condition to obtain activated ore pulp;
s2: separating the activated ore pulp by using a hydrocyclone to obtain coal slime water and a solid slag phase;
s3: measuring a hydrogen peroxide solution according to the volume ratio of the coal slime water to the first hydrogen peroxide solution of 1: 1-3, uniformly mixing the coal slime water and the hydrogen peroxide solution, performing supercritical treatment, cooling and standing, and obtaining supernatant and lower-layer sludge.
Compared with the prior art, the invention has the beneficial effects that:
the coal slime water cleaning method provided by the invention comprises the steps of firstly, activating crushed and ground coal gangue under the supercritical or subcritical water condition to reduce the chemical stability of minerals, and converting crystal form into amorphous state to improve the activity; passing through the waterThe strong centrifugal acting force of the cyclone is utilized to separate an organic liquid phase and a solid slag phase, so that the primary separation of minerals is realized; mixing the organic liquid phase and the hydrogen peroxide solution, reacting for 30-90 min in a supercritical environment at 220-300 ℃ and 15-40 MPa, and cooling and standing the obtained mixed solution to enable the coal slime to quickly sink to the bottom. The invention adopts supercritical treatment after adding hydrogen peroxide to achieve the purpose of quickly treating the slime water, and the method has simple operation, does not consume a large amount of medicines, does not need any catalyst, is not influenced by the water quality, and has better water quality after treatment. The cleaning method of the invention realizes the rapid cleaning of the slime water, and by utilizing the supercritical water advanced oxidation treatment technology, organic matters in the slime water are rapidly oxidized and decomposed into carbon dioxide and water under the high temperature and high pressure of oxygen decomposed by hydrogen peroxide in a supercritical medium, the obtained supernatant liquid has high cleanliness and can be directly discharged, and the settled waste residue can be used as organic fertilizer mud and can also be directly discharged. The core of the invention lies in the property of supercritical water (the dielectric constant is reduced to be similar to that of organic matters and gas, so that the gas and the organic matters can be completely dissolved in water to form a homogeneous oxidation system), the activity is higher, the reaction rate is improved, the reaction is complete, and organic carbon and hydrogen are completely converted into CO2And H2And O. Compared with the prior art, the invention has the advantages of high treatment efficiency, thorough damage to toxic pollutants, no introduction of other impurities and quick reaction. In addition, harmful chemical agents are not required to be added, only high-temperature and high-pressure thermal decomposition is carried out, and hydrogen peroxide is decomposed into water and oxygen, so that the method is environment-friendly and has no chemical pollution.
Through detection, the COD content of the water treated by the method is reduced to 23mg/L, and the water completely meets the national four-class water use standards, such as domestic water for bathing, swimming pools and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a diagram of a matter treated by a method of cleaning slime water in example 1;
FIG. 2 is a diagram of a material object treated by the method for cleaning slime water in example 2;
FIG. 3 is a diagram of a material object treated by the method for cleaning slime water in example 3;
FIG. 4 is a diagram of a substance treated by the method of cleaning slime water in example 4.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the technical solutions in the embodiments of the present invention may be combined with each other, but it must be based on the realization of those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination of technical solutions should not be considered to exist, and is not within the protection scope of the present invention.
The drugs/reagents used are all commercially available without specific mention.
The invention provides a method for cleaning slime water, which comprises the following steps:
s1: and performing activation treatment on the crushed and ground coal gangue under the subcritical or supercritical water condition to obtain activated ore pulp.
Preferably, the activation treatment is specifically: activating the crushed and ground coal gangue at 250-400 ℃ and 8-20 MPa for 0.1-3 h. Under the subcritical or supercritical water condition, the chemical stability of the mineral is reduced by activating under the subcritical or supercritical water condition, and the crystal form transformation is carried out to convert into an amorphous state so as to improve the activity.
Preferably, the activation treatment is specifically: and uniformly mixing the crushed and ground coal gangue with a second aqueous solution of hydrogen peroxide, and activating for 0.1-3 h under the subcritical or supercritical water condition of 250-400 ℃ and 8-20 MPa. The hydrogen peroxide is used as an oxidant, so that the oxidation activation efficiency of subcritical or supercritical water can be obviously improved.
Preferably, the mass ratio of the coal gangue to the second aqueous solution of hydrogen peroxide is 1: 1-1.5. If the ratio is less than 1:1, the concentration of the mineral decomposition is too high, the reaction is difficult to be sufficient, and the activation effect is not good. If >1:1.5, the activation effect is improved to some extent but is not significant, and the control is not more than 1.5 for economic reasons. The purpose of adding hydrogen peroxide is mainly to improve the activation efficiency, reduce the chemical stability of minerals, realize the primary separation of minerals and simultaneously realize the purpose of treating part of easily degradable organic matters.
The concentration of hydrogen peroxide in the second hydrogen peroxide solution is 1-10%. The aim is to enhance the activation efficiency of the coal gangue, and considering commercial cost and actual reaction effect, the optimal concentration of the hydrogen peroxide is less than 10%, the activation reaction effect is not obvious when the concentration is too low, and the cost is too high when the concentration is too high.
Preferably, the size of the crushed and ground coal gangue is 75-500 μm. From the activation purpose, the mineral with the particle size of more than 500 mu m is difficult to activate, the time consumption is long, the fine particles with the particle size of less than 75 mu m are too many, the concentration of the sludge which is difficult to treat in the waste liquid is too high, and the treatment cost is high, so the preferable particle size is 75-500 mu m.
S2: and separating the activated ore pulp by using a hydrocyclone to obtain coal slime water and a solid slag phase. The slime water is an organic liquid phase containing fine particle slime.
Preferably, the diameter of an overflow port of the hydrocyclone is 30mm, the diameter of a sand settling port of the hydrocyclone is 20mm, and the overall height of the hydrocyclone is 761.5 mm. A suitable hydrocyclone was chosen for better separation.
Preferably, the pressure of the hydrocyclone is controlled to be 0.1-0.3 MPa. In order to make the working state of the cyclone optimum, the sorting effect is obvious. The working principle of the cyclone is centrifugal sedimentation, the larger the pressure is, the larger the centrifugal force is, so that most of fine mud minerals are discharged from an overflow port, the pressure is not selected to be lower than 0.1MPa, and meanwhile, if the pressure is too large, the flow of the overflow port is too large, overflow products are mixed, the separation effect of coarse particles and fine particles is not good, and therefore, the pressure is controlled to be lower than 0.3 MPa.
S3: measuring a hydrogen peroxide solution according to the volume ratio of the coal slime water to the first hydrogen peroxide solution of 1: 1-3, uniformly mixing the coal slime water and the hydrogen peroxide solution, performing supercritical treatment, cooling and standing, and obtaining supernatant and lower-layer sludge.
Preferably, the concentration of the hydrogen peroxide in the first hydrogen peroxide solution is 5-10%. Aims to deeply treat organic matters in the coal slime wastewater and purify water quality. If the concentration of the hydrogen peroxide is lower than 5%, OH generated by hydrogen peroxide is less, so that the oxidation efficiency of organic matters is seriously influenced, and if the concentration of the hydrogen peroxide is higher than 10%, on one hand, the waste of the hydrogen peroxide is caused, the cost is increased, and on the other hand, the residual hydrogen peroxide in the solution is also a problem to be treated.
Preferably, the volume ratio of the coal slime water to the first hydrogen peroxide solution is 1: 2. The purpose is to fully react with organic matters in the coal slime wastewater, and simultaneously play a role in diluting the coal slime. The coal slurry wastewater from the overflow port of the cyclone has high organic matter content and high concentration, simultaneously carries a large amount of coal slurry, and can purify the water quality only by diluting and fully contacting the coal slurry, so the volume ratio of the coal slurry water to the first hydrogen peroxide solution is selected to be 1: 2.
Preferably, the supercritical treatment temperature is 220-300 ℃, the pressure is 15-40 MPa, and the time is 30-90 min.
Example 1
The embodiment provides a method for cleaning slime water, which comprises the following steps:
s1: crushing and grinding coal gangue to 75 μm, uniformly mixing the crushed and ground coal gangue with a second aqueous solution of hydrogen peroxide with the concentration of 5% according to a ratio of 1:1.2, activating for 30min under the subcritical water condition of 320 ℃ and 8MPa to obtain activated ore pulp, and dissociating most of minerals after activation.
S2: and separating the activated ore pulp by using a hydrocyclone to obtain coal slime water and a solid slag phase.
The diameter of an overflow port of the hydrocyclone is 30mm, the diameter of a sand settling port is 20mm, and the overall height of the hydrocyclone is 761.5 mm. The pressure of the hydraulic cyclone is controlled at 0.2 Mpa.
S3: measuring a hydrogen peroxide solution with the concentration of 5% according to the volume ratio of 1:1 of the coal slime water to the first hydrogen peroxide solution, uniformly mixing the coal slime water and the hydrogen peroxide solution, putting the mixture into a reaction kettle at the temperature of 220 ℃ for supercritical treatment, wherein the supercritical pressure is 25MPa, treating for 60min, cooling and standing, and obtaining supernatant and lower-layer sludge as shown in figure 1. As can be seen from FIG. 1, the cleaning method provided by the present invention can be used to clean the slime water quickly. The method is used for treating the slime water, and the influence of chemical agents such as flocculating agent and the like on the environment is avoided.
Example 2
The embodiment provides a method for cleaning slime water, which comprises the following steps:
s1: crushing and grinding coal gangue to 75 μm, uniformly mixing the crushed and ground coal gangue with a second aqueous solution of hydrogen peroxide with the concentration of 1% according to a ratio of 1:1.5, activating for 60min under the subcritical water condition of 250 ℃ and 15MPa to obtain activated ore pulp, and dissociating most of minerals after activation.
S2: and separating the activated ore pulp by using a hydrocyclone to obtain coal slime water and a solid slag phase.
The diameter of an overflow port of the hydrocyclone is 30mm, the diameter of a sand settling port is 20mm, and the overall height of the hydrocyclone is 761.5 mm. The pressure of the hydraulic cyclone is controlled at 0.1 Mpa.
S3: measuring a hydrogen peroxide solution with the concentration of 5% according to the volume ratio of 1:1 of the coal slime water to the first hydrogen peroxide solution, uniformly mixing the coal slime water and the hydrogen peroxide solution, putting the mixture into a reaction kettle at the temperature of 260 ℃ for supercritical treatment, wherein the supercritical pressure is 25MPa, treating for 60min, cooling and standing, and obtaining supernatant and lower-layer sludge as shown in figure 2. As can be seen from FIG. 2, the cleaning method provided by the present invention can be used to clean the slime water quickly. The method is used for treating the slime water, and the influence of chemical agents such as flocculating agent and the like on the environment is avoided.
Example 3
The embodiment provides a method for cleaning slime water, which comprises the following steps:
s1: crushing and grinding coal gangue to 75 μm, uniformly mixing the crushed and ground coal gangue with a second aqueous solution of hydrogen peroxide with the concentration of 10% according to a ratio of 1:1, activating for 6min under the subcritical water condition of 400 ℃ and 20MPa to obtain activated ore pulp, and dissociating most of minerals after activation.
S2: and separating the activated ore pulp by using a hydrocyclone to obtain coal slime water and a solid slag phase.
The diameter of an overflow port of the hydrocyclone is 30mm, the diameter of a sand settling port is 20mm, and the overall height of the hydrocyclone is 761.5 mm. The pressure of the hydraulic cyclone is controlled at 0.3 Mpa.
S3: measuring a hydrogen peroxide solution with the concentration of 5% according to the volume ratio of 1:1 of the coal slime water to the first hydrogen peroxide solution, uniformly mixing the coal slime water and the hydrogen peroxide solution, putting the mixture into a reaction kettle at the temperature of 280 ℃ for supercritical treatment, wherein the supercritical pressure is 25MPa, treating for 60min, cooling and standing, and obtaining supernatant and lower-layer sludge as shown in figure 3. As can be seen from FIG. 3, the cleaning method provided by the present invention can be used to clean the slime water quickly. The method is used for treating the slime water, and the influence of chemical agents such as flocculating agent and the like on the environment is avoided.
Example 4
The embodiment provides a method for cleaning slime water, which comprises the following steps:
s1: crushing and grinding coal gangue to 75 μm, uniformly mixing the crushed and ground coal gangue with a second aqueous solution of hydrogen peroxide with the concentration of 5% according to a ratio of 1:1.2, activating for 30min under the subcritical water condition of 320 ℃ and 8MPa to obtain activated ore pulp, and dissociating most of minerals after activation.
S2: and separating the activated ore pulp by using a hydrocyclone to obtain coal slime water and a solid slag phase.
The diameter of an overflow port of the hydrocyclone is 30mm, the diameter of a sand settling port is 20mm, and the overall height of the hydrocyclone is 761.5 mm. The pressure of the hydraulic cyclone is controlled at 0.2 Mpa.
S3: measuring a hydrogen peroxide solution with the concentration of 5% according to the volume ratio of 1:2 of the coal slime water to the first hydrogen peroxide solution, uniformly mixing the coal slime water and the hydrogen peroxide solution, putting the mixture into a reaction kettle at the temperature of 220 ℃ for supercritical treatment, wherein the supercritical pressure is 25MPa, treating for 60min, cooling and standing, and obtaining supernatant and lower-layer sludge as shown in figure 4. As can be seen from FIG. 4, the cleaning method provided by the present invention can be used to clean the slime water quickly. The method is used for treating the slime water, and the influence of chemical agents such as flocculating agent and the like on the environment is avoided.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A method for cleaning slime water is characterized by comprising the following steps:
s1: performing activation treatment on the crushed and ground coal gangue under the subcritical or supercritical water condition to obtain activated ore pulp;
s2: separating the activated ore pulp by using a hydrocyclone to obtain coal slime water and a solid slag phase;
s3: measuring a hydrogen peroxide solution according to the volume ratio of the coal slime water to the first hydrogen peroxide solution of 1: 1-3, uniformly mixing the coal slime water and the hydrogen peroxide solution, performing supercritical treatment, cooling and standing, and obtaining supernatant and lower-layer sludge.
2. The method for cleaning coal slime water as claimed in claim 1, wherein in step S1, the activation treatment is specifically:
and activating the crushed and ground coal gangue for 0.1-3 h under the subcritical or supercritical water condition of 250-400 ℃ and 8-20 MPa.
3. The method for cleaning coal slime water as claimed in claim 1, wherein in step S1, the activation treatment is specifically:
and uniformly mixing the crushed and ground coal gangue with a second aqueous solution of hydrogen peroxide, and activating for 0.1-3 h under the subcritical or supercritical water condition of 250-400 ℃ and 8-20 MPa.
4. The method for cleaning the coal slime water as claimed in claim 3, wherein the mass ratio of the coal gangue to the second hydrogen peroxide solution is 1: 1-1.5; the concentration of hydrogen peroxide in the second hydrogen peroxide solution is 1-10%.
5. The method for cleaning the coal slime water as set forth in any one of claims 1 to 3, wherein in the step S1, the size of the crushed and ground coal gangue is 75 to 500 μm.
6. The method for cleaning the coal slime water as set forth in claim 1, wherein in step S2, the overflow port of the hydrocyclone has a diameter of 30mm, the sand settling port has a diameter of 20mm, and the whole height of the hydrocyclone is 761.5 mm.
7. The method for cleaning the coal slime water as set forth in claim 1 or 6, wherein the pressure of the hydrocyclone is controlled to be 0.1-0.3 MPa.
8. The method for cleaning the coal slime water as set forth in claim 1, wherein in step S3, the concentration of hydrogen peroxide in the first hydrogen peroxide solution is 5-10%.
9. The method for cleaning the coal slurry as claimed in claim 1, wherein the volume ratio of the coal slurry to the first hydrogen peroxide solution is 1:2 in step S3.
10. The method for cleaning the coal slime water as set forth in claim 1, wherein in step S3, the supercritical treatment temperature is 220-300 ℃, the pressure is 15-40 MPa, and the time is 30-90 min.
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Application publication date: 20220329 |