CN110947358A - Preparation method and application method of underground water remediation agent - Google Patents
Preparation method and application method of underground water remediation agent Download PDFInfo
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- CN110947358A CN110947358A CN201911036475.5A CN201911036475A CN110947358A CN 110947358 A CN110947358 A CN 110947358A CN 201911036475 A CN201911036475 A CN 201911036475A CN 110947358 A CN110947358 A CN 110947358A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
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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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
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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
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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
- C02F2103/06—Contaminated groundwater or leachate
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Abstract
The invention discloses a preparation method and an application method of an underground water remediation medicament, which are respectively characterized in that 20 parts of attapulgite are ground and sieved by a 200-mesh sieve, and are mixed with 100 parts of hydrochloric acid; stirring for 40 minutes at the constant temperature of 30 ℃, then carrying out ultrasonic treatment for 20 minutes, standing for 20 minutes after the ultrasonic treatment is finished, and obtaining a premix; and washing the premix to be neutral and drying at 105 ℃ to obtain the attapulgite mixture. The preparation method of the underground water remediation medicament provided by the invention overcomes the defects that the existing underground water remediation medicament is generally a chemical preparation or is complex in components and cannot be recycled, and provides an application method of the underground water remediation medicament, which can adsorb inorganic and organic pollutants in underground water, can be recycled, realizes resource utilization, harmlessness and conservation in the underground water remediation process, and has important social and economic benefits.
Description
Technical Field
The invention relates to the technical field of groundwater remediation, in particular to a preparation method and an application method of a groundwater remediation agent.
Background
In 2018, the published' 2017 publication of ecological environment conditions in China, such as Weijian Commission of the national Weijian and the national transformation Commission, the proportion of the national groundwater with the water quality of better grade or above is only 33.4%, and the worse grade and the worst grade respectively reach 51.8% and 14.8%. The tap water turns yellow and is mixed with impurities, and thick water scale is generated at the bottom of the kettle when the kettle is used for boiling the water for a long time; well water in some rural areas is not sweet and clear any more, but is turbid and slightly bitter, even has peculiar smell, and the obvious manifestation of groundwater pollution in life is realized. But which contaminants are contained in the groundwater and cannot be seen with the naked eye. The underground water is slow in circulation, weak in self-cleaning capacity and poor in pollution condition. From 'Chinese environmental condition bulletin' of the past years, the total ratio of the worse grade and the extreme difference grade of the underground water is increased from 55% of 2011 to 66.6% of 2017, and the ratio of the good grade, the good grade and the good grade water is not increased. The groundwater pollution prevention program 2011-Bu 2020 shows that about 61% of urban residents in China use groundwater as a drinking water source; in northern areas 65% of domestic water, 50% of industrial water and 33% of agricultural irrigation water are from groundwater. Once the groundwater is polluted, the harm is the aspect of life. Therefore, the method enhances the prevention and treatment of the uncontaminated underground water and the remediation work of the contaminated underground water, and has important practical significance for guaranteeing the drinking water safety, harmony between people and nature, and comprehensive, harmonious and sustainable development of the economy and the society.
Attapulgite, called attapulgite (palygorskite) for short, is attapulgite clay ore with a layer chain transition structure and mainly containing water-containing magnesium-rich silicate, and is widely regarded in the fields of clay mineral science, material science, physical chemistry, soil science, environmental engineering, archaeology and the like. In 1976, China discovers attapulgite ores in Liuhe small mountain of Jiangsu province and the like for the first time, and then discovers large-scale attapulgite ores in Suwan region, particularly mountain streams and Guanshan mountain areas of Ming City of Anhui province, and the proven ore reserves, the grades and the annual mining scale all occupy the top of the world. According to the estimation, the storage capacity of the attapulgite in China accounts for more than 50% of the total storage capacity of the world, and the attapulgite is a high-quality mineral deposit in the world and has great development value. The adsorptivity of attapulgite depends on its large specific surface area, surface physicochemical structure and its ionic state, and its adsorption includes physical adsorption, chemical adsorption and ion exchange adsorption. The attapulgite has good adsorption effect on organic matters, heavy metals, ammonia nitrogen, nitrate nitrogen and the like, the modified attapulgite has improved purity, improved surface activity and enlarged specific surface area, and is more beneficial to water retention and fertilizer retention and adsorption of pollutants in soil.
Most of the components of the existing underground water remediation agents are chemical agents or the proportion of the components is complex, and the underground water is related to the safety of drinking water of residents, so that pollution-free agents are selected to be safer during remediation.
Disclosure of Invention
The invention aims to provide a preparation method and an application method of an underground water remediation medicament, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of an underground water remediation agent comprises the following steps:
the method comprises the following steps: grinding 20 parts of attapulgite, sieving with a 200-mesh sieve, and mixing with 100 parts of hydrochloric acid;
step two: stirring for 40 minutes at the constant temperature of 30 ℃, then carrying out ultrasonic treatment for 20 minutes, standing for 20 minutes after the ultrasonic treatment is finished, and obtaining a premix;
step three: and washing the premix to be neutral and drying at 105 ℃ to obtain the attapulgite mixture.
The concentration of the hydrochloric acid is 2 mol/L.
An application method of a groundwater remediation medicament comprises the following steps:
the method comprises the following steps: extracting polluted underground water into a sewage treatment system through a pumping well, and adding an attapulgite mixture into the sewage treatment system;
step two: the sewage treatment system is internally provided with a temperature control device and a stirring device, the environmental temperature of the system is kept at 30 ℃, and the stirring speed is 180 r/min;
step three: and (3) detecting the water quality change in real time on line in the adsorption process, closing a water inlet valve of the sewage treatment system and opening a water outlet valve after adsorption is balanced, and discharging and refluxing the treated underground water to the underground.
The water pumping wells are arranged in a plurality of rows, and the arrangement density is 400 square meters per square meter.
The adding proportion of the attapulgite mixture is 2-20Kg/m3。
And the adsorption time in the third step is 60-90 min.
In step three, the attapulgite mixture is separated by a sedimentation tank before refluxing to the ground, and the pH value is adjusted to 6.5-7.5.
The adding proportion of the attapulgite mixture is 8Kg/m3。
And the adsorption time in the third step is 90 min.
According to the technical scheme, the preparation method of the underground water remediation medicament overcomes the defects that the existing underground water remediation medicament is generally a chemical preparation or is complex in components and cannot be recycled, provides the application method of the underground water remediation medicament, can adsorb inorganic and organic pollutants in underground water, can be recycled, realizes reclamation, harmlessness and conservation in the underground water remediation process, and has important social and economic benefits.
Drawings
FIG. 1 is an infrared spectrum of a hydrochloric acid modified sepiolite according to the invention;
FIG. 2 is an infrared spectrum of bentonite according to the invention;
FIG. 3 is an infrared spectrum of an attapulgite according to the present invention;
FIG. 4 is an XRD pattern of hydrochloric acid modified sepiolite according to the invention;
FIG. 5 is an XRD pattern of a hydrochloric acid modified bentonite according to the invention;
FIG. 6 is an XRD pattern of a hydrochloric acid modified attapulgite according to the present invention;
FIG. 7 is a schematic view showing the effect of different adsorption times on adsorption rates of modified attapulgite and unmodified attapulgite in accordance with the present invention;
FIG. 8 is a schematic diagram showing the effect of different adsorption pH values on adsorption rates of modified attapulgite and unmodified attapulgite in accordance with the present invention;
FIG. 9 is a schematic diagram showing the effect of different adsorption amounts of modified attapulgite and unmodified attapulgite on the adsorption rate according to the present invention.
Detailed Description
In order to verify the optimal mineral and hydrochloric acid concentration selected from the hydrochloric acid-modified silicate minerals, the following protocol was used, and the treatment marks are shown in table one;
(watch one)
The method comprises the following implementation steps:
the method comprises the following steps: weighing 20g (200 meshes) of attapulgite, bentonite and sepiolite, placing the attapulgite, the bentonite and the sepiolite into a beaker, marking, respectively adding 100mL of hydrochloric acid of 0.1mol/L, 0.5mol/L, 1mol/L, 2mol/L and 4mol/L, stirring at constant temperature of 30 ℃ for 40min, carrying out ultrasonic treatment for 20min, standing for 20min, centrifuging for multiple times, washing the solid to be neutral by deionized water, drying at 105 ℃, grinding, sealing and storing for later use;
step two: measuring BET surface area and pore size;
measuring the specific surface area of sepiolite, bentonite, attapulgite and modified hydrochloric acid by using a Tristar II 3020 specific surface area and pore size determinator produced by MICROMERICIS;
step three: infrared spectroscopy (FTIR);
carrying out infrared spectrum analysis on samples modified by sepiolite, bentonite, attapulgite and hydrochloric acid by using a nicolet 670FT-IR type infrared spectrometer produced by the company of thermo in America;
step four: x-ray diffraction analysis (XRD);
the specific surface area and the aperture of the sample are measured by a Rigaku ultima IV ray spectrometer produced by Rigaku Raman company in America;
the results of the changes of the specific surface area and the pore diameter after modification are shown in the following table II:
(watch two)
After hydrochloric acid modification, the specific surface areas of the three clay minerals are increased and then reduced, when the concentration of acid reaches 2.0mol/L, the specific surface area value is increased to the maximum, the specific surface area of sepiolite is enlarged by more than 9 times, and the specific surface area of attapulgite is enlarged by 2.5 times, compared with the prior art, the modification effect of bentonite is not obvious and is only 1.7 times. In general, the attapulgite, whether unmodified or modified, has a specific surface area far greater than that of sepiolite and bentonite, which is related to the structure of the attapulgite, and the structural characteristics of the attapulgite are internal porous channels, surface grooves, specific surface area and porosity. When the acid concentration is increased to 4mol/L, the specific surface area of each clay mineral begins to decrease, which means that the acid modification concentration is not too large, and the best effect is achieved by 2mol/L hydrochloric acid.
Fourier transform Infrared Spectroscopy (FTIR) analysis results are shown in FIGS. 1-3;
after the modification treatment by hydrochloric acid, the impurity carbonate of sepiolite, bentonite and attapulgite is obviously reduced, the purity is improved, and the change of the absorption peak after the modification treatment when the concentration of hydrochloric acid is 2mol/L is more obvious. In general, the attapulgite has higher component purity than sepiolite and bentonite before and after modification.
Probing the change of the modified clay mineral structure by using X-ray, and obtaining the results shown in FIGS. 4-6;
and (3) exploring the change of the modified clay mineral structure by using X rays, wherein the change of the attapulgite structure is large. A characteristic diffraction peak of an ATP (111) crystal face at a 2 theta of 30.95 DEG, which is weakened when AATP of a hydrochloric acid concentration of 1mol/L appears, and disappears when AATP treated with hydrochloric acid of 2mol/L appears; the absorption peak appearing at a 2 theta of 32.92 degrees disappears after ATP treatment; absorption peaks at 41.41 DEG and 45.17 DEG in terms of 2 theta disappear at a hydrochloric acid concentration of 1mol/L following hydrochloric acid treatment. Shows that the components of the attapulgite are changed by the modification of the hydrochloric acid. The reason may be that dolomite impurity components appear at 30.95 °, 32.92 °, 41.41 ° and 45.17 ° 2 θ, and the dolomite rises with the addition of hydrochloric acid. The purpose of this change is, of course, to obtain a larger specific surface area, to widen the pores in the crystal structure and to enhance the attapulgite activity.
The test shows that: the 2mol/L hydrochloric acid has the best modification effect, wherein the purity of the modified attapulgite is improved, the surface activity is improved, the specific surface area is enlarged, and the modification effect is better than that of sepiolite and bentonite.
Secondly, in order to determine the optimal adsorption condition for repairing polluted underground water by the modified attapulgite, the following tests are carried out:
(1) test groundwater: selecting underground water to be repaired polluted in a certain place according to a grade III standard in an underground water quality standard (GB/T14848-2017), wherein the components in the underground water are shown in the following table III;
(TABLE III) (mg/L)
(2) Selection of optimum adsorption time: respectively weighing 2g of modified attapulgite (A) and unmodified attapulgite (B), adding 250mL of sewage into a 500mL conical flask, uniformly mixing, adjusting the pH to 5 by NaOH, setting the temperature to be 30 ℃, oscillating and adsorbing at 180r/min, setting the adsorption time to be 10min, 20min, 30min, 40min, 50min, 60min, 90min and 120min, centrifugally separating, measuring the pollutant value in the supernatant, and calculating the removal rate by using a differential subtraction method.
(3) The adsorption rates of the modified attapulgite (A) and the unmodified attapulgite (B) are increased in the first 50min of adsorption, and the adsorption rate of the modified attapulgite is higher than that of the unmodified attapulgite. When the adsorption time is 60min, the adsorption rate of the unmodified attapulgite is 0, which indicates that the adsorption saturation is achieved, while the adsorption rate of the modified attapulgite is still slowly increased until the adsorption equilibrium is achieved within 90min, as shown in table four and fig. 7;
(watch four)
FIG. 7 shows the effect of different adsorption times on adsorption rates.
(4) Optimal adsorption pH selection: respectively weighing 2g of modified attapulgite (A) and unmodified attapulgite (B), adding 250mL of sewage into a 500mL conical flask, uniformly mixing, adjusting the pH by using hydrochloric acid and NaOH, setting the pH to be 7 gradients, setting the pH to be 1, 2, 3, 4, 5, 6 and 7, setting the temperature to be 30 ℃, oscillating and adsorbing for 90min at 180r/min, after centrifugal separation, measuring the pollutant value in the supernatant, and calculating the removal rate by using a differential method.
(5) With the increase of the pH, the change curve of the adsorption rate of the attapulgite shows a trend of ascending first and then descending, which reflects that the attapulgite has an adsorption-desorption process under the influence of the pH, under the condition of lower pH, the adsorption rate of the attapulgite is low, the adsorption rate is gradually increased along with the increase of the pH, when the pH reaches 5, the adsorption rate reaches the maximum, and the pH is increased, but the adsorption rate is reduced, which indicates that the attapulgite starts to desorb at the moment, as shown in the fifth table and fig. 8;
(watch five)
FIG. 8 shows the effect of different adsorption pH values on the adsorption rate.
(6) Selection of optimal adsorption dosage: respectively weighing 0.5g, 1g, 1.5g, 2g, 2.5g, 5g of modified attapulgite (A) and unmodified attapulgite (B) into a 500mL conical flask, adding 250mL of sewage, uniformly mixing, adjusting the pH to 5 by using hydrochloric acid and NaOH, setting the temperature to be 30 ℃, oscillating and adsorbing for 90min at 180r/min, after centrifugal separation, measuring the pollutant value in the supernatant, and calculating the removal rate by using a differential subtraction method.
(7) Influence of the adsorption amount on the adsorption effect of the modified attapulgite. The results showed that the adsorption rate of the modified attapulgite for each pollutant (COD, NH4-N, NO3-N, Pb) in the wastewater increased with the increase of the adsorption amount, and when the addition amount reached 2g, the adsorption rate of the modified attapulgite increased to the maximum and the adsorption equilibrium was reached.
The adsorption rate of the unmodified attapulgite also increases along with the increase of the adsorption dosage, and when the addition amount is 2g, the adsorption rate tends to slowly increase, but the adsorption rate is lower than that of the modified attapulgite, so that the adsorption capacity of the modified attapulgite is higher than that of the unmodified attapulgite under the condition of the same addition amount, as shown in Table six and FIG. 9;
(watch six)
Wherein, fig. 9 shows the effect of different adsorption amounts on the adsorption rate.
The following conclusions can be drawn through the verification of the examples above:
(1) the silicic acid mineral is modified by the hydrochloric acid, the specific surface area of the attapulgite is increased, the components are purified, and the modification effect is better than that of sepiolite and bentonite. The concentration of the modified hydrochloric acid is 2 mol/L.
(2) The best condition for adsorbing underground water pollutants by the modified attapulgite is that the adsorption amount is 8Kg/m3The adsorption pH is 5, the adsorption time is 90min, the modified attapulgite can adsorb inorganic pollutants, has strong adsorption capacity on organic pollutants in underground water, and the treated underground water has COD (chemical oxygen demand)MnThe removal rate is 82%, the removal rate of NH4-N is 85%, the removal rate of NO3-N is 82%, and the removal rate of Pb reaches 87%.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (9)
1. The preparation method of the underground water restoration agent is characterized by comprising the following steps:
the method comprises the following steps: grinding 20 parts of attapulgite, sieving with a 200-mesh sieve, and mixing with 100 parts of hydrochloric acid;
step two: stirring for 40 minutes at the constant temperature of 30 ℃, then carrying out ultrasonic treatment for 20 minutes, standing for 20 minutes after the ultrasonic treatment is finished, and obtaining a premix;
step three: and washing the premix to be neutral and drying at 105 ℃ to obtain the attapulgite mixture.
2. The method for preparing an underground water remediation agent as claimed in claim 1, wherein: the concentration of the hydrochloric acid is 2 mol/L.
3. A method of using an agent for groundwater remediation according to any of claims 1 to 2 including the steps of:
the method comprises the following steps: extracting polluted underground water into a sewage treatment system through a pumping well, and adding an attapulgite mixture into the sewage treatment system;
step two: the sewage treatment system is internally provided with a temperature control device and a stirring device, the environmental temperature of the system is kept at 30 ℃, and the stirring speed is 180 r/min;
step three: and (3) detecting the water quality change in real time on line in the adsorption process, closing a water inlet valve of the sewage treatment system and opening a water outlet valve after adsorption is balanced, and discharging and refluxing the treated underground water to the underground.
4. The method for using an underground water remediation agent as claimed in claim 3, wherein: the water pumping wells are arranged in a plurality of rows, and the arrangement density is 400 square meters per square meter.
5. The method for using an underground water remediation agent as claimed in claim 3, wherein: the adding proportion of the attapulgite mixture is 2-20Kg/m3。
6. The method for using an underground water remediation agent as claimed in claim 3, wherein: and the adsorption time in the third step is 60-90 min.
7. The method for using an underground water remediation agent as claimed in claim 3, wherein: in step three, the attapulgite mixture is separated by a sedimentation tank before refluxing to the ground, and the pH value is adjusted to 6.5-7.5.
8. The method for applying an underground water remediation agent as claimed in claim 5, wherein: the adding proportion of the attapulgite mixture is 8Kg/m3。
9. The method for using an underground water remediation agent as claimed in claim 6, wherein: and the adsorption time in the third step is 90 min.
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Address after: No. 3966, Qimen Road, Baohe District, Hefei, Anhui Province, 230009 Applicant after: ANHUI TONGYUAN ENVIRONMENT ENERGY SAVING Co.,Ltd. Address before: No. 856, Jinzhai South Road, Baohe District, Hefei City, Anhui Province, 230041 Applicant before: ANHUI TONGYUAN ENVIRONMENT ENERGY SAVING Co.,Ltd. |
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Application publication date: 20200403 |