CN111115785A - Method for repairing mercury-polluted underground water - Google Patents
Method for repairing mercury-polluted underground water Download PDFInfo
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- CN111115785A CN111115785A CN202010005157.9A CN202010005157A CN111115785A CN 111115785 A CN111115785 A CN 111115785A CN 202010005157 A CN202010005157 A CN 202010005157A CN 111115785 A CN111115785 A CN 111115785A
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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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal 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
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Abstract
The invention discloses a method for repairing mercury-polluted underground water, which treats and repairs the mercury-polluted underground water by using a CMC-FeS nano material as an in-situ reaction zone, and comprises the following steps: and (4) loading the column by a wet method, penetrating and intercepting the nano material, and immobilizing the mercury by the intercepted nano material. The CMC-FeS nano material has controllable transmission behavior in a saturated porous medium and can be injected into a pollution depth and a pollution position; an effective reaction zone formed in an underground environment can be used for efficiently immobilizing mercury; the invention provides a novel underground water in-situ remediation method, which has a wide application prospect in underground water in-situ remediation.
Description
Technical Field
The invention belongs to the technical field of underground water treatment, and relates to a method for repairing mercury-polluted underground water, in particular to a method for repairing mercury-polluted underground water by using a sodium carboxymethylcellulose (CMC) -stabilized ferrous sulfide (FeS) (CMC-FeS) nano material as an in-situ reaction zone.
Background
Groundwater is an important component of water resources and plays an important role in the development of natural ecosystems and human survival. With the rapid development of human society, various industrial activities, such as metal smelting, chlor-alkali industry, mining, coal combustion and other industrial wastewater discharge into the environment cause groundwater mercury pollution. Mercury is a heavy metal with high toxicity and bioaccumulation. The long-time exposure to the mercury pollution environment can cause damage to the central nervous system and renal failure of human bodies, and the like, thereby causing threat to human health. The treatment and remediation of mercury pollution of underground water become one of the key points and difficulties of environmental remediation.
Ferrous sulfide (FeS) is a natural sulfur mineral that immobilizes mercury in the environment through the mechanisms of chemical precipitation, ion exchange and surface complexation. However, FeS, either naturally occurring or prepared by traditional methods, tends to agglomerate, is typically on the order of millimeters or larger in particle size, is not soil-transportable, cannot be injected into the underground environment, and limits its immobilization effect on mercury.
At present, In-situ remediation technologies for groundwater are increasingly applied to treatment of polluted groundwater, and mainly include Permeable Reactive Barrier (PRB) and In-situ reactive zone (IRZ) remediation technologies. The in-situ reaction zone repairing technology is a novel underground water in-situ repairing method developed based on a permeable reaction wall repairing technology, namely, a proper reaction reagent is injected into an underground water environment through an injection well to create one or more in-situ reaction zones, and pollutants are intercepted and fixed, so that the aim of repairing underground water pollution is fulfilled.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention provides the method for repairing the mercury-polluted underground water by using the CMC-FeS nano material as the in-situ reaction zone.
The purpose of the invention is realized by the following technical scheme:
a method for repairing mercury-polluted underground water specifically comprises the following steps:
(1) preparing a CMC-FeS nano material: mixing CMC: FeSO4：Na2S is prepared from the following components in a mixed solution system according to the mass concentration of (1-4.17): 5.27: 4.55 preparation, under the protection of nitrogen, FeSO4The solution is added to CMC water solution to form Fe2 +CMC complex, nitrogen venting for 10min, drippingAdding Na2S, obtaining a CMC-FeS nano material;
(2) injecting the CMC-FeS nano material prepared in the step (1) into a porous medium glass column filled by a wet method, and monitoring the concentration of the CMC-FeS nano material in the effluent liquid in real time until the concentration of the CMC-FeS nano material in the effluent liquid is kept unchanged to form a CMC-FeS in-situ reaction zone;
(3) and (3) injecting the mercury-polluted underground water into the CMC-FeS in-situ reaction zone in the step (2), receiving samples at the outlet of the reaction device every 1 hour, measuring the concentration of mercury in effluent liquid until the concentration of mercury is kept unchanged, and finishing the whole repair work of the mercury-polluted underground water.
Preferably, the CMC in the preparation of the CMC-FeS nanomaterial in the step (1) is: FeSO4：Na2S is mixed with the mixed solution system according to the mass concentration ratio of 1.67: 5.27: 4.55 configuration.
Preferably, the injection concentration of the CMC-FeS nano-material in the step (2) is 100 mg/L-300 mg/L.
Preferably, the injection flow rate of the CMC-FeS nano-material in the step (2) is 0.02mL/min to 0.06 mL/min.
Preferably, the porous medium in the step (2) is quartz sand with a mesh size of 40-80 meshes.
Preferably, the injection flow rate of the mercury-polluted underground water in the step (3) is 0.02mL/min to 0.06 mL/min.
Preferably, the concentration of mercury in the effluent is measured by atomic fluorescence spectrophotometry in the step (3).
The working principle of the invention is as follows:
an In situ reactive zone (IRZ) repairing technology is a novel underground water In-situ repairing method developed on the basis of a Permeable Reactive Barrier (PRB) repairing technology, namely, a proper reaction reagent is injected into an underground water environment through an injection well to create one or more In-situ reaction zones, and pollutants are trapped and fixed, so that the aim of repairing underground water pollution is fulfilled.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the CMC-FeS nano material has controllable transmission behavior in a saturated porous medium and can be injected into a pollution depth and a pollution position; an effective reaction zone formed in an underground environment can be used for efficiently immobilizing mercury;
(2) the method adopts an In-situ reactive zone (IRZ) repairing technology, has small environmental disturbance, does not need to excavate a polluted area, and reduces the risk of human body exposure; the repairing effect is good, the contact surface of the pollutants and the repairing material is larger, the reaction time is longer, and the repairing effect is better; the restoration range is not limited by the depth of the polluted feather, and the method can be used for the treatment and restoration of deep polluted groundwater; the construction equipment is simple, and the repair cost is low.
Drawings
FIG. 1 is a schematic diagram of the apparatus of the present invention;
FIG. 2 is a graph of the effect of injection flow velocity on the breakthrough behavior of CMC-FeS in a saturated silica sand column in example 2;
FIG. 3 is a graph of the effect of initial concentration of nanomaterials on the penetration behavior of CMC-FeS in a saturated silica sand column in example 3;
FIG. 4 is a graph showing the effect of groundwater flow velocity on the effect of immobilized mercury in the CMC-FeS in situ reaction zone in example 4;
FIG. 5 is a graph of the effect of initial mercury concentration on the immobilized mercury effect of the CMC-FeS in-situ reaction zone in example 5;
fig. 6 is a comparison of the effect of the CMC-FeS nanomaterial in-situ reaction zone repair technique and the CMC-FeS nanomaterial permeable reaction wall repair technique on mercury immobilization in example 6.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
Experimental materials in this example:
sodium carboxymethylcellulose (CMC), ferrous sulfide (FeSO)4) Sodium sulfide (Na)2S), hydrochloric acid (HCL), mercury pollute groundwater.
Example 1: preparation of CMC-FeS nano material and determination of mixture ratio
(1) Preparing a CMC-FeS nano material: adding 100mg CMC into 170ml water to prepare CMC solution, adding nitrogen gas (A), (B), (C), (>99%) exhausting gas to the CMC solution for 20min to remove dissolved oxygen in the solution; 20mL of 15.8g/L FeSO4The solution is added to CMC water solution to form Fe2+CMC complex, nitrogen bleed gas: (>99%) for 10min, 10mL of 27.3g/L Na is added dropwise2S solution to obtain CMC-FeS, CMC and FeSO with the mass concentration of 500mg/L in the mixed solution system of the three4And Na2The mass ratio of S is 1.67: 5.27: 4.55 of CMC-FeS nano material. Adjusting the amount of CMC, wherein CMC and FeSO4And Na2The mass concentration ratio of S is (1-4.17): 5.27: 4.55 CMC-FeS nano materials with different proportions are respectively configured.
It was found that FeSO was obtained according to the above experimental method4The solution is added to CMC water solution to form Fe2+-CMC complex, Na added dropwise2And (4) reacting the S solution to prepare the CMC-FeS nano material. In a mixture solution system, when CMC and FeSO4When the mass concentration ratio of (2) is 0.2, the prepared FeS is completely stable, suspended in the solution and has soil transferability. When in a mixture system, CMC and FeSO4When the mass concentration ratio of the mercury is more than or equal to 0.2, the mercury-free remediation catalyst can be applied to an in-situ reaction zone to restore mercury-polluted underground water. Wherein, in the mixture solution system, CMC and FeSO4The mass concentration ratio of (3) to (3) is 0.2, the CMC-FeS particle diameters are 253, 223 and 166nm, respectively, and the adsorption capacities to Hg are 2805, 2800 and 2408mg/g, respectively.
In the following examples 2 to 6, CMC and FeSO were selected in a mixture solution system4The mass concentration ratio is 1.67: 5.27 Experimental investigations were carried out.
Preparing a CMC-FeS nano material with the mass concentration of 100mg/L in a mixture solution system: adding 20mg of CMC into 170ml of water to prepare CMC solution, and then adding nitrogen (C)>99%) exhausting gas to the CMC solution for 20min to remove dissolved oxygen in the solution; 20mL of 3.16g/L FeSO4The solution is added to a CMC aqueous solutionIn (1), Fe is formed2+CMC complex, nitrogen bleed gas: (>99%) for 10min, 10mL of 5.46g/L Na are added dropwise2And (5) preparing an S solution.
Preparing a CMC-FeS nano material with the mass concentration of 300mg/L in a mixture solution system: 60mg of CMC was added to 170ml of water to prepare a CMC solution, and nitrogen was used (>99%) exhausting gas to the CMC solution for 20min to remove dissolved oxygen in the solution; 20mL of 9.48g/L FeSO4The solution is added to CMC water solution to form Fe2+CMC complex, nitrogen bleed gas: (>99%) for 10min, 10mL of 16.38g/L Na are added dropwise2And (5) preparing an S solution.
Example 2: influence of injection speed on penetration behavior of CMC-FeS nano material in saturated porous medium
(1) The porous medium is selected from quartz sand of 40-80 meshes, metal oxides and dust on the surface of the quartz sand are cleaned through steps of water washing, acid washing and the like, and the quartz sand is naturally dried for later use. Injecting the CMC-FeS nano material with the mass concentration of 100mg/L prepared in the embodiment 1 into a saturated quartz sand column;
(2) weighing 0.2g of glass wool, and compacting at the bottom of the organic glass column; weighing 13.5g of quartz sand, and filling the quartz sand into an organic glass column by adopting a wet packing method; connecting an injection pump, a glass column and an automatic part collector by using a polytetrafluoroethylene tube (PTFE tube), and keeping the whole system in a closed state; injecting the CMC-FeS nano material into the sand column from the top end of the sand column and flowing out from the bottom of the sand column; the flow rates of the CMC-FeS nano material in the injection pump are respectively set to be 0.02mL/min and 0.06 mL/min. Monitoring the concentration of the nano material in the effluent in real time until the concentration of the nano material in the effluent is basically kept unchanged;
(3) injecting a background solution simulating underground water into an organic glass column by using an injection pump for elution, and measuring the concentration of the nano material in an effluent until the concentration is basically zero;
(4) the samples were collected with an automatic fraction collector for a preset time (20 min samples before one hour, followed by 10min samples after a reduction in time, 8 samples were collected, and the subsequent time was set to 1 hour each.) and were dissolved with 12M HCl (the volume ratio of the sample to hydrochloric acid was 1:4), and after 5min of reaction, the solubility of Fe in the solution was measured by flame atomic absorption spectrophotometry.
The breakthrough curves of the CMC-FeS nanomaterials in a saturated silica sand column at different injection rates are shown in fig. 2. When the flow rate is 0.02mL/min, C/C0The value of (A) is 0.97, and the interception amount of the nano material in the saturated quartz sand is 0.042 mg; when the flow rate is 0.06mL/min, C/C0The value of (A) is 0.98. By changing the flow rate of the CMC-FeS nano material, the low injection speed is beneficial to the interception of the CMC-FeS nano material in the quartz sand column.
Example 3: effect of initial Mass concentration of nanomaterials on the penetration behavior of CMC-FeS in saturated Quartz Sand columns
(1) Experimental reactor set-up as in figure 1, experimental reactor set-up preparation method as in example 2;
(2) the CMC-FeS nano material is injected into a glass column filled with quartz sand by a syringe pump, the injection speed is set to be 0.06mL/min, the CMC-FeS nano material prepared in the embodiment 1 is taken, and the initial mass concentration is 100mg/L and 300mg/L respectively. Monitoring the concentration of the nano material in the effluent in real time until the concentration of the nano material in the effluent is basically kept unchanged;
(3) background solution simulating groundwater was injected into the glass column with a syringe pump for elution. Measuring the concentration of the nanomaterial in the effluent until the nanomaterial concentration is substantially zero;
(4) the samples were collected with an automatic fraction collector at a preset time (20 min samples before one hour, followed by 10min samples after a reduction time, and the subsequent time was set to 1 hour), dissolved in 12M HCl (volume ratio of sample to concentrated HCl 1:4), and after 5min of reaction, the solubility of Fe in the solution was measured by flame atomic absorption spectrophotometry.
The effect of the initial concentration of the nanomaterial on the penetration behavior of CMC-FeS in a column of saturated quartz sand is shown in fig. 3. When the concentration of the nano material is increased from 100mg/L to 300mg/L, C/C0Increases the value of (c) from 0.98 to 1.0. The experimental results show that the higher the concentration of the nano material is, the easier the nano material is eluted from the quartz sand.
Example 4: influence of groundwater flow velocity on immobilized mercury effect of CMC-FeS in-situ reaction zone
(1) Experimental reactor set-up as in figure 1, experimental reactor set-up preparation method as in example 2;
(2) obtaining an in-situ reaction zone of the CMC-FeS nano-material according to the operation steps in the embodiment 2, wherein the injection speed of a precision injection pump is 0.06mL/min, the initial mass concentration of the CMC-FeS nano-material prepared in the embodiment 1 is 300mg/L, and the interception amount in a quartz sand column is 0.096 mg;
(3) injecting polluted underground water containing mercury (the concentration of mercury is 600 mug/L) into a CMC-FeS in-situ reaction zone system by using a precision injection pump, wherein the set flow rates are 0.02mL/min and 0.06mL/min respectively;
(4) sampling was performed for a predetermined period of time (one sample was set to 1 hour), and the concentration of mercury in the effluent was measured by atomic fluorescence spectrophotometry.
FIG. 4 shows the effect of typical groundwater flow velocity on the effect of immobilized mercury in the CMC-FeS in situ reaction zone. When the flow rate was increased from 0.02mL/min to 0.06mL/min, the mercury removal rate decreased from 58.82% to 55.24%.
Example 5: influence of initial concentration of mercury on immobilized mercury effect of CMC-FeS in-situ reaction zone
(1) Experimental reactor set-up as in figure 1, experimental reactor set-up preparation method as in example 2;
(2) obtaining an in-situ reaction zone of the CMC-FeS nano-material according to the operation steps in the embodiment 2, wherein the injection speed of a precision injection pump is 0.06mL/min, the initial mass concentration of the CMC-FeS nano-material prepared in the embodiment 1 is 300mg/L, and the interception amount in a quartz sand column is 0.096 mg;
(3) injecting the mercury-containing polluted underground water into a glass column filled with quartz sand by using an injection pump, wherein the injection speed is set to be 0.06mL/min, and the concentration of the mercury-containing polluted underground water is set to be 100 mu g/L and 600 mu g/L;
(4) sampling was performed for a predetermined period of time (one sample was set to 1 hour), and the concentration of mercury in the effluent was measured by atomic fluorescence spectrophotometry.
FIG. 5 compares the effect of initial mercury concentration on the effect of immobilized mercury in CMC-FeS in situ reaction zone. When the initial concentration of mercury is increased from 100 mug/L to 600 mug/L, the removal rate of mercury is respectively reduced from 78.19 percent to 55.24 percent.
Example 6: comparison of CMC-FeS nanomaterial in-situ reaction zone repair technology and CMC-FeS nanomaterial permeable reaction wall repair technology on mercury immobilization effect
(1) Experimental reactor set-up as in figure 1, experimental reactor set-up preparation method as in example 2;
(2) weighing 0.2g of glass wool, and compacting at the bottom of the organic glass column; weighing 0.096mg of CMC-FeS particles and 13.5g of quartz sand, and filling into an organic glass column by a wet packing method; connecting an injection pump, a glass column and an automatic part collector by using a polytetrafluoroethylene tube (PTFE tube), and keeping the whole system in a closed state;
(3) injecting polluted underground water containing mercury (the concentration of mercury is 600 mug/L) into a CMC-FeS permeable reaction wall system by using a precise injection pump, wherein the set injection flow rate is 0.06 mL/min;
(4) sampling was performed for a predetermined period of time (one sample was set to 1 hour), and the concentration of mercury in the effluent was measured by atomic fluorescence spectrophotometry.
As can be seen from fig. 6, the removal rate of the CMC-FeS PRB repair technology to mercury is 9.52%, which is much lower than the mercury immobilization effect of the CMC-FeS in-situ reaction zone (the removal rate of mercury is 55.24%).
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. The method for repairing the mercury-polluted underground water is characterized by comprising the following steps:
(1) preparing a CMC-FeS nano material: mixing CMC: FeSO4：Na2S is prepared from the following components in a mixed solution system according to the mass concentration of (1-4.17): 5.27: 4.55 configuration, under the protection of nitrogen, theFeSO4The solution is added to CMC water solution to form Fe2+-CMC complex, venting nitrogen for 10min, adding Na dropwise2S, obtaining a CMC-FeS nano material;
(2) injecting the CMC-FeS nano material prepared in the step (1) into a porous medium glass column filled by a wet method, and monitoring the concentration of the CMC-FeS nano material in the effluent liquid in real time until the concentration of the CMC-FeS nano material in the effluent liquid is kept unchanged to form a CMC-FeS in-situ reaction zone;
(3) and (3) injecting the mercury-polluted underground water into the CMC-FeS in-situ reaction zone in the step (2), receiving samples at the outlet of the reaction device every 1 hour, measuring the concentration of mercury in effluent liquid until the concentration of mercury is kept unchanged, and finishing the whole repair work of the mercury-polluted underground water.
2. The method for remediating mercury-contaminated groundwater according to claim 1, wherein the CMC in the CMC-FeS nanomaterial preparation in the step (1) is: FeSO4：Na2S is mixed with the mixed solution system according to the mass concentration ratio of 1.67: 5.27: 4.55 configuration.
3. The method for remediating mercury-contaminated groundwater according to claim 1, wherein the injection concentration of the CMC-FeS nanomaterial in the step (2) is 100mg/L to 300 mg/L.
4. The method for remediating mercury-contaminated groundwater according to claim 1, wherein the CMC-FeS nanomaterial injection flow rate in the step (2) is 0.02mL/min to 0.06 mL/min.
5. The method for remediating mercury-contaminated groundwater as claimed in claim 1, wherein the porous medium in the step (2) is quartz sand of 40-80 meshes.
6. The method for remediating mercury-contaminated groundwater according to claim 1, wherein the injection flow rate of mercury-contaminated groundwater in the step (3) is 0.02mL/min to 0.06 mL/min.
7. The method for remediating mercury-contaminated groundwater as claimed in claim 1, wherein the concentration of mercury in the effluent is measured in the step (3) using atomic fluorescence spectrophotometry.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116037632A (en) * | 2022-11-21 | 2023-05-02 | 南开大学 | Method for in-situ reconstruction of underground aquifer and application |
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| JPS58224134A (en) * | 1982-06-22 | 1983-12-26 | Seitetsu Kagaku Co Ltd | Method for recovering mercury from waste water |
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| CN116037632A (en) * | 2022-11-21 | 2023-05-02 | 南开大学 | Method for in-situ reconstruction of underground aquifer and application |
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Application publication date: 20200508 |