CN112934204A - Heavy metal mercury adsorbent and preparation method thereof - Google Patents
Heavy metal mercury adsorbent and preparation method thereof Download PDFInfo
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- CN112934204A CN112934204A CN202110201096.8A CN202110201096A CN112934204A CN 112934204 A CN112934204 A CN 112934204A CN 202110201096 A CN202110201096 A CN 202110201096A CN 112934204 A CN112934204 A CN 112934204A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0211—Compounds of Ti, Zr, Hf
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28011—Other properties, e.g. density, crush strength
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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
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses a heavy metal mercury (Hg) adsorbent and a preparation method thereof, belongs to the technical field of heavy metal wastewater treatment, and provides a heavy metal mercury adsorbent. The heavy metal mercury adsorbent prepared by the method has super-strong stability, excellent stability of acid resistance, alkali resistance and organic solvent resistance, can be used as an efficient and stable heavy metal mercury adsorption material, has high heavy metal Hg (II) adsorption capacity and high adsorption kinetics rate, can remove heavy metal Hg (II) in an aqueous solution from a complex water body in a targeted manner, and has excellent recycling performance.
Description
Technical Field
The invention belongs to the technical field of heavy metal wastewater treatment, and particularly relates to a heavy metal mercury adsorbent and a preparation method thereof.
Background
Among the heavy metals, mercury (hg (ii)) has a broad transmission pathway, extremely strong toxicity and bioaccumulation, and its environmental exposure poses a great hazard to the ecological environment and human health. However, the mercury-containing wastewater has various types, complicated water quality conditions, complicated treatment process and difficulty in realizing deep removal. Therefore, the development of a high-efficiency mercury removal technology in a water body has important significance for improving the wastewater treatment efficiency, meeting the requirement of advanced treatment on mercury-containing wastewater in key industries and protecting the water quality safety and the human health.
Adsorption technology has long been used to treat heavy metal pollution in water because of its high efficiency, simplicity and low cost. However, the traditional adsorption materials including zeolite, activated carbon, silica gel, clay, etc. cannot meet increasingly complex water environment pollution and increasingly strict water quality standards due to low adsorption affinity, small adsorption capacity and poor adsorption selectivity. Therefore, the development of new high-efficiency mercury adsorption materials is urgent.
Disclosure of Invention
The invention aims to provide a heavy metal mercury adsorbent and a preparation method thereof, the adsorbent material has good stability, excellent acid and alkali resistance and organic solvent resistance, high adsorption capacity, small influence of solution acid and alkali, capability of realizing rapid and efficient targeted removal of Hg (II) in water, good recycling effect, easy separation and suitability for large-scale engineering application.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a heavy metal mercury adsorbent, which takes porous melamine sponge as a matrix, and stably loads Zr-MSA nano particles inside the porous melamine sponge by utilizing the strong hydrogen bond action between polyvinylidene fluoride (PVDF) net films and the Zr-MSA nano particles.
In a preferable scheme, the loading amount of Zr-MSA on the melamine sponge matrix is 30-40 wt%.
More preferably, the loading amount of the Zr-MSA on the melamine sponge matrix is 35-40 wt%.
The invention also provides a preparation method of the heavy metal mercury adsorbent, which comprises the following steps:
(1) preparing Zr-MSA nano particles;
(2) preparing a Zr-MSA/PVDF/DMF ternary mixed solution:
adding Zr-MSA nano particles into a DMF solvent, carrying out ultrasonic treatment by using a cell disruptor to obtain a Zr-MSA/DMF mixed solution, then heating and stirring, slowly adding PVDF powder into the Zr-MSA/DMF mixed solution, and uniformly stirring to obtain a Zr-MSA/PVDF/DMF ternary mixed solution;
(3) preparation of heavy metal mercury adsorbent:
dipping melamine sponge in Zr-MSA/PVDF/DMF ternary mixed solution, taking out the sponge after repeated extrusion and draining the dispersion liquid adhered to the surface; and (3) drying the soaked melamine sponge at a preset temperature, and cooling the melamine sponge to room temperature by using an oven to obtain the heavy metal mercury adsorbent.
Preferably, in the step (1), the preparation process of the Zr-MSA nanoparticles is as follows:
s1, mixing ZrCl4Dissolving the mixture and mercaptomalic acid in deionized water according to a set ratio, and performing ultrasonic treatment to obtain a mixed solution;
s2, adding formic acid into the mixed solution obtained in the step S1, uniformly mixing, transferring the obtained solution into a closed container, and placing the closed container at a preset temperature for reaction;
s3, cooling the mixed solution in the closed container to room temperature, centrifugally separating the obtained white precipitate, washing and drying to obtain the Zr-MSA nano-particles.
Further, in step S1, ZrCl4The mass ratio of the compound to the mercaptomalic acid is 23.3 (15-18.75).
Further, in step S2, the formic acid is ZrCl4The addition amount of (B) is 55-70 wt%.
Further, in step S2, the reaction temperature is 60-100 ℃ and the reaction time is 2-4 h.
Preferably, in the step (2), the heating and stirring temperature is 40-60 ℃.
In the preferable scheme, in the step (3), the soaked melamine sponge is kept for 2-4 hours at 120-180 ℃.
The invention designs a method for preparing a stable heavy metal mercury adsorbent by an impregnation-phase separation method, which comprises the following steps: the preparation method comprises the steps of selecting Zr-MSA as a load object, dipping melamine sponge into PVDF/Zr-MSA/DMF mixed dispersion liquid, and then repeatedly extruding to enable the mixed dispersion liquid to be well dispersed in the melamine sponge. And finally, heating the melamine sponge fully filled with the mixed dispersion liquid to solidify the inert PVDF with low surface energy on the surfaces of the Zr-MSA particles and the fiber bundles in the melamine sponge to form the porous membrane. The PVDF porous membrane can form hydrogen bond acting force with Zr-MSA particles while coating the Zr-MSA particles and fiber bundles, so that the effect of stably fixing the Zr-MSA particles by a net is realized.
According to the heavy metal mercury adsorbent, the Zr-MSA nanoparticles subjected to ultrasonic dispersion are stably loaded on the porous melamine sponge by means of the strong hydrogen bond action between the PVDF net film and the Zr-MSA nanoparticles. The heavy metal mercury adsorbent disclosed by the invention utilizes abundant sulfydryl adsorption sites, porosity and large specific surface area of Zr-MSA, and realizes efficient selective targeted removal of Hg (II).
The preparation method of the heavy metal mercury adsorbent is simple to operate, mild in working condition and has the potential of large-scale actual production. The heavy metal mercury adsorbent prepared by the invention has the advantages of strong stability, good adsorption effect, easy recovery, repeated recycling, and larger practical value and engineering application prospect.
The technical scheme of the invention has the following beneficial effects:
(1) the method can uniformly disperse the loaded Zr-MSA nano particles on the internal fiber bundles of the low-cost porous melamine sponge, and the PVDF film generated by phase separation can fix the Zr-MSA particles on the internal fiber bundles of the sponge, so that the problems of easy agglomeration and difficult recovery of the Zr-MSA nano particles are solved, and the problem of secondary pollution caused by leakage of Zr-MSA powder is effectively avoided.
(2) The heavy metal mercury adsorbent prepared by the invention has higher Hg (II) adsorption capacity, and can quickly and deeply remove Hg (II) in an aqueous solution; in addition, the heavy metal mercury adsorbent prepared by the invention has excellent acid and alkali resistance influence capacity and coexisting cation interference resistance capacity, can realize targeted removal of Hg (II) under complex environmental conditions, and has a high practical application value.
(3) The heavy metal mercury adsorbent disclosed by the invention keeps better stability and Hg (II) removal effect after being placed in acid, alkali and various organic solvents with various concentrations for 3 months respectively. After 25 times of adsorption cycles, the heavy metal mercury adsorbent still has excellent Hg (II) removal efficiency, which is the recycling performance which is difficult to achieve by the existing Hg (II) adsorbent, and has higher economic value.
Drawings
Fig. 1 is a photographic view of the heavy metal mercury sorbent prepared in example 3.
Fig. 2 is an SEM image of the heavy metal mercury sorbent prepared in example 3.
Fig. 3 is an XRD pattern of Zr-MSA nanoparticles prepared in example 1 and heavy metal mercury sorbent prepared in example 3.
Fig. 4 is an adsorption isotherm curve of the heavy metal mercury sorbent prepared in example 3 for removal of hg (ii).
Fig. 5 is an adsorption kinetics curve of the heavy metal mercury adsorbent prepared in example 3 for removing hg (ii).
Fig. 6 is a graph of the effect of solution initial pH on hg (ii) removal by the heavy metal mercury sorbent prepared in example 3.
Fig. 7 is a graph of the effect of coexisting cations on hg (ii) removal by the heavy metal mercury sorbent prepared in example 3.
FIG. 8 shows the stability tests of the heavy metal mercury adsorbents prepared in example 3 after soaking in different solvents for 3 months (A is tap water, B, C, D is 0.1mol/L, 1mol/L and 6mol/L HCl solutions, E, F is 1mmol/L and 10mmol/L NaOH solutions, and G, H, I, J is dimethylformamide, dimethyl sulfoxide, dichloromethane and ethanol, respectively).
Fig. 9 is a graph of the cycle effect of the heavy metal mercury sorbent prepared in example 3 for removing hg (ii).
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by those skilled in the art without any creative work based on the embodiments of the present invention belong to the protection scope of the present invention.
The invention is further illustrated below with reference to specific embodiments and the accompanying drawings.
Example 1: preparation of Zr-MSA nanoparticles
23.3g of ZrCl4Dissolving 15g of mercaptomalic acid (MSA) in 200mL of deionized water, and adding 13mL of formic acid into the solution after carrying out ultrasonic treatment for 1 minute; covering a bottle cap, and placing the solution in an oven at 80 ℃ for reaction for 3 hours; and after cooling to room temperature, centrifugally separating the obtained white precipitate, washing with deionized water for 4 times, and freeze-drying for 24 hours to obtain the Zr-MSA nano-particles.
Example 2: preparation of Zr-MSA/PVDF/DMF ternary mixed solution
2g of Zr-MSA powder obtained in example 1 is taken to be dispersed in 100ml of mixed solution of DMF, stirred for 5min and ultrasonically treated for 15min by using a cell disruptor (1200w) under the ice bath condition to ensure that Zr-MSA particles are highly dispersed; under the condition of heating and stirring at 50 ℃, 2g of PVDF powder is slowly added into the Zr-MSA/DMF mixed solution, and the Zr-MSA/PVDF/DMF ternary mixed solution which is uniformly dispersed is obtained after magnetic stirring for 2 hours.
Example 3: preparation of heavy metal mercury adsorbent
Cutting off melamine sponge (1.5 × 1.5 × 5 cm)3) Dipping in Zr-MSA/PVDF/DMF ternary mixed solution obtained in example 2, repeatedly extruding for 5 times, taking out sponge and draining dispersion liquid adhered to the surface; and (3) putting the soaked melamine sponge into an electric heating constant-temperature drying oven, heating to 150 ℃, keeping for 3h, and cooling the drying oven to room temperature to obtain the high-stability heavy metal mercury adsorbent Zr-MSA/PVDF @ MS. Through testing, heavy metal mercury absorbsThe loading of Zr-MSA nano particles in the additive is about 37.0 wt%.
Fig. 1 is a photograph of the heavy metal mercury sorbent prepared in example 3, the heavy metal mercury sorbent prepared by the above method having a light yellow appearance.
Fig. 2 is an SEM image of the heavy metal mercury sorbent prepared in example 3, with Zr-MSA nanoparticles uniformly distributed on the inner fiber bundle of the heavy metal mercury sorbent prepared by the above method.
FIG. 3 is an XRD pattern of Zr-MSA nanoparticles prepared in example 1 and a heavy metal mercury adsorbent Zr-MSA/PVDF @ MS prepared in example 3, the Zr-MSA/PVDF @ MS shows an X-ray diffraction pattern spectrum similar to that of Zr-MSA, and the Zr-MSA nanoparticles retain the original crystallinity and crystal form after being loaded by the method.
Example 4: isothermal adsorption experiment (static adsorption experiment for adsorption Performance test)
40mL of Hg (II) solutions with initial concentrations of 50mg/L, 100mg/L, 150mg/L, 250mg/L, 300mg/L, 350mg/L, 450mg/L and 500mg/L are respectively added into a centrifuge tube, the pH value is adjusted to 3.0 by hydrochloric acid solution or sodium hydroxide solution, 20mg of heavy metal mercury adsorbent Zr-MSA/PVDF @ MS is added, the centrifuge tube is placed in a constant temperature air bath shaker at 25 ℃ and is shaken for 24 hours at the rotating speed of 180 r/min. After the static adsorption experiment was completed, 2mL of the solution was removed and filtered through a 0.22 μm filter, and the concentration of the remaining Hg (II) was measured by inductively coupled plasma mass spectrometry (ICP-MS), and the adsorption capacity was calculated from the results.
Fig. 4 is an adsorption isotherm curve of the heavy metal mercury sorbent prepared in example 3 for removal of hg (ii). The result shows that the adsorption of the heavy metal mercury adsorbent obtained by the invention to Hg (II) is more in line with a Langmuir adsorption model, the heavy metal mercury adsorbent belongs to monolayer chemical adsorption, and the theoretical maximum adsorption capacity is 353.2 mg/g.
Example 5: adsorption kinetics experiment
Adding 100mL of Hg (II) solution with the initial concentration of 10000 mug/L into a conical flask, adjusting the pH to 3.0 by using a hydrochloric acid solution or a sodium hydroxide solution, adding 100mg of a heavy metal mercury adsorbent Zr-MSA/PVDF @ MS, placing a centrifugal tube into a constant-temperature air bath shaking table with the rotation speed of 180r/min and the temperature of 25 ℃, taking 1mL of reaction liquid when the reaction time is 1min, 5min, 15min, 30min, 60min and 120min respectively, filtering the reaction liquid by using a 0.22 mu m filter membrane, and measuring the residual Hg (II) concentration at the corresponding time by using ICP-MS.
Fig. 5 is an adsorption kinetics curve of the heavy metal mercury adsorbent prepared in example 3 for removing hg (ii). The result shows that the heavy metal mercury adsorbent prepared by the method has an ultra-fast Hg (II) adsorption rate, can remove more than 96.9 percent of Hg (II) in 15min, and finally realizes the fast deep removal of Hg (II) with the residual Hg (II) concentration lower than 1 mu g/L.
Example 6: experiment of influence of pH on solution
Adding 12 parts of 40mL Hg (II) solution with the initial concentration of 10000 mu g/L into a centrifuge tube, respectively adjusting the pH to 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11 and 12 by using hydrochloric acid solution or sodium hydroxide solution, adding 40mg of heavy metal mercury adsorbent Zr-MSA/PVDF @ MS, and placing the centrifuge tube in a constant-temperature air bath shaking table with the rotation speed of 180r/min and the temperature of 25 ℃ for shaking for 4 hours. After completion of the adsorption experiment, 1mL of the reaction solution was filtered through a 0.22 μm filter and the remaining Hg (II) concentration of each pH solution was measured by ICP-MS.
Fig. 6 is a graph of the effect of solution initial pH on hg (ii) removal by the heavy metal mercury sorbent prepared in example 3.
The result shows that the heavy metal mercury adsorbent prepared by the invention can remove more than 99.0 percent of Hg (II) in the pH range of 2-10, and has excellent capacity of resisting the influence of solution acid and alkali.
Example 7: coexisting cation interference experiments
Na (I), K (I), Ca (II), Mg (II), Pb (II), Cu (II), Cd (II), Ni (II), Zn (II) and Mix (Mix' indicates that 9 cations exist simultaneously) are respectively added into 40mL of Hg (II) solution containing 10000 mug/L, then 40mg of heavy metal mercury adsorbent Zr-MSA/PVDF @ MS is added, and the centrifuge tube is placed in a constant temperature air bath shaking table with the rotating speed of 180r/min and the temperature of 25 ℃ for oscillation for 4 h. After completion of the adsorption experiment, 1mL of the reaction solution was taken out, filtered through a 0.22 μm filter, and the remaining Hg (II) concentration in each solution was measured by ICP-MS.
Fig. 7 is a graph of the effect of coexisting cations on hg (ii) removal by the heavy metal mercury sorbent prepared in example 3. The result shows that the heavy metal mercury adsorbent prepared by the invention has excellent capacity of resisting the interference of coexisting cations, the removal rate is over 99.9% under the condition that 9 interference cations exist respectively, and the removal rate is still over 98.9% under the condition that 9 cations exist simultaneously.
Example 8: solvent corrosion stability test
Respectively placing a certain weight of heavy metal mercury adsorbent into glass bottles filled with different solvents, extruding to fully soak the heavy metal mercury adsorbent in the solvents, standing and soaking for 3 months, taking out, drying and recording the weight. The rate of change in weight was calculated using the following formula: mass change ratio (m)0-m)/m0) X 100% where m0And m is the weight (g) of the heavy metal mercury sorbent before and after the solvent soaking process, respectively.
FIG. 8 shows the stability tests of the heavy metal mercury adsorbents prepared in example 3 after soaking in different solvents for 3 months (A is tap water, B, C, D is 0.1mol/L, 1mol/L and 6mol/L HCl solutions, E, F is 1mmol/L and 10mmol/L NaOH solutions, and G, H, I, J is dimethylformamide, dimethyl sulfoxide, dichloromethane and ethanol, respectively). The result shows that the heavy metal mercury adsorbent disclosed by the invention keeps better stability and Hg (II) removal effect after being respectively placed in acid, alkali and organic solvents with various concentrations for 3 months.
Example 9: test for cycling stability
100mL of an initial solution of 10000. mu.g/L of Hg (II) were added to a conical flask, the pH was adjusted to 3.0, 100mg of the MOF-based sponge adsorbent Zr-MSA/PVDF @ MS were added, and the tube was shaken for 4h in a thermostatted air-bath shaker at 25 ℃ and a rotation speed of 180 r/min. After the static adsorption experiment was completed, 2mL of the solution was taken out to determine the residual concentration. And (3) recovering the heavy metal mercury adsorbent by filtering, washing with deionized water for 3 times, placing in a drying box at 60 ℃, drying, entering the next round of adsorption experiment, and performing a cycle experiment for 25 times.
Fig. 9 is a graph of the cycle effect of the heavy metal mercury sorbent prepared in example 3 for removing hg (ii). The result shows that the heavy metal mercury adsorbent still has excellent Hg (II) removal efficiency after being recycled for 25 times, which is the recycling performance which is difficult to achieve by the existing Hg (II) adsorbent, and has higher economic value.
Claims (10)
1. The heavy metal mercury adsorbent is characterized in that porous melamine sponge is used as a matrix, and Zr-MSA nanoparticles are stably loaded inside the porous melamine sponge by utilizing the strong hydrogen bond effect between a polyvinylidene fluoride net film and the Zr-MSA nanoparticles.
2. The heavy metal mercury sorbent according to claim 1, wherein the loading of the Zr-MSA on the melamine sponge matrix is 30-40 wt%.
3. The heavy metal mercury sorbent according to claim 2, wherein the loading of the Zr-MSA on the melamine sponge matrix is 35-40 wt%.
4. The method for preparing a heavy metal mercury sorbent according to any one of claims 1 to 3, comprising the steps of:
(1) preparing Zr-MSA nano particles;
(2) preparing a Zr-MSA/PVDF/DMF ternary mixed solution:
adding Zr-MSA nano particles into a DMF solvent, carrying out ultrasonic treatment by using a cell disruptor to obtain a Zr-MSA/DMF mixed solution, then heating and stirring, slowly adding PVDF powder into the Zr-MSA/DMF mixed solution, and uniformly stirring to obtain a Zr-MSA/PVDF/DMF ternary mixed solution;
(3) preparation of heavy metal mercury adsorbent:
dipping melamine sponge in Zr-MSA/PVDF/DMF ternary mixed solution, taking out the sponge after repeated extrusion and draining the dispersion liquid adhered to the surface; and (3) drying the soaked melamine sponge at a preset temperature, and cooling the melamine sponge to room temperature by using an oven to obtain the heavy metal mercury adsorbent.
5. The preparation method of the heavy metal mercury sorbent according to claim 4, wherein in the step (1), the preparation process of the Zr-MSA nanoparticles is as follows:
s1, mixing ZrCl4Dissolving the mixture and mercaptomalic acid in deionized water according to a set ratio, and performing ultrasonic treatment to obtain a mixed solution;
s2, adding formic acid into the mixed solution obtained in the step S1, uniformly mixing, transferring the obtained solution into a closed container, and placing the closed container at a preset temperature for reaction;
s3, cooling the mixed solution in the closed container to room temperature, centrifugally separating the obtained white precipitate, washing and drying to obtain the Zr-MSA nano-particles.
6. The method for preparing the heavy metal mercury sorbent of claim 5, wherein in step S1, the ZrCl is added4The mass ratio of the compound to the mercaptomalic acid is 23.3 (15-18.75).
7. The method for preparing the heavy metal mercury sorbent according to claim 5, wherein the formic acid is ZrCl relatively in step S24The addition amount of (B) is 55-70 wt%.
8. The method for preparing a heavy metal mercury sorbent according to claim 5, wherein in the step S2, the reaction temperature is 60-100 ℃ and the reaction time is 2-4 h.
9. The method for preparing the heavy metal mercury sorbent according to claim 4, wherein the heating and stirring temperature in the step (2) is 40-60 ℃.
10. The preparation method of the heavy metal mercury sorbent according to claim 4, wherein in the step (3), the soaked melamine sponge is kept at 120-180 ℃ for 2-4 h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115282785A (en) * | 2022-09-30 | 2022-11-04 | 天津工业大学 | MXene composite adsorption film and preparation method thereof |
| CN115582102A (en) * | 2022-10-08 | 2023-01-10 | 湖南大学 | Porous sponge adsorbent and preparation method and application thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1336241A (en) * | 1970-02-05 | 1973-11-07 | Osaka Soda Co Ltd | Purification process |
| CN105148852A (en) * | 2015-10-12 | 2015-12-16 | 武汉大学 | Thiohydroxy-modified magnetic MOFs adsorbent and preparation method and application thereof |
| EP3227017A2 (en) * | 2014-12-04 | 2017-10-11 | Numat Technologies Inc. | Porous polymers for the abatement and purification of electronic gas and the removal of mercury from hydrocarbon streams |
| CN109317104A (en) * | 2018-11-02 | 2019-02-12 | 北京工业大学 | A kind of mercapto-functionalized metal-organic framework materials, preparation and its application |
| CN109926031A (en) * | 2019-04-04 | 2019-06-25 | 北京工业大学 | A kind of MOFs/ sponge composite material and preparation method and application |
| CN110283328A (en) * | 2019-05-28 | 2019-09-27 | 江汉大学 | A kind of zirconium metal-organic framework material and preparation method thereof as crystal sponge |
| CN112295603A (en) * | 2020-09-30 | 2021-02-02 | 浙江理工大学 | Preparation method, product and application of ultra-stable MOFs-based porous sponge |
-
2021
- 2021-02-23 CN CN202110201096.8A patent/CN112934204A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1336241A (en) * | 1970-02-05 | 1973-11-07 | Osaka Soda Co Ltd | Purification process |
| EP3227017A2 (en) * | 2014-12-04 | 2017-10-11 | Numat Technologies Inc. | Porous polymers for the abatement and purification of electronic gas and the removal of mercury from hydrocarbon streams |
| CN105148852A (en) * | 2015-10-12 | 2015-12-16 | 武汉大学 | Thiohydroxy-modified magnetic MOFs adsorbent and preparation method and application thereof |
| CN109317104A (en) * | 2018-11-02 | 2019-02-12 | 北京工业大学 | A kind of mercapto-functionalized metal-organic framework materials, preparation and its application |
| CN109926031A (en) * | 2019-04-04 | 2019-06-25 | 北京工业大学 | A kind of MOFs/ sponge composite material and preparation method and application |
| CN110283328A (en) * | 2019-05-28 | 2019-09-27 | 江汉大学 | A kind of zirconium metal-organic framework material and preparation method thereof as crystal sponge |
| CN112295603A (en) * | 2020-09-30 | 2021-02-02 | 浙江理工大学 | Preparation method, product and application of ultra-stable MOFs-based porous sponge |
Non-Patent Citations (1)
| Title |
|---|
| PENGFEI YANG ET AL.: "A robust MOF-based trap with high-density active alkyl thiol for the super-efficient capture of mercury", 《CHEMICAL COMMUNICATIONS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115282785A (en) * | 2022-09-30 | 2022-11-04 | 天津工业大学 | MXene composite adsorption film and preparation method thereof |
| CN115582102A (en) * | 2022-10-08 | 2023-01-10 | 湖南大学 | Porous sponge adsorbent and preparation method and application thereof |
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