CN111729662A - Preparation method and application of MXene membrane material for in-situ growth of Bi-MOF - Google Patents
Preparation method and application of MXene membrane material for in-situ growth of Bi-MOF Download PDFInfo
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- CN111729662A CN111729662A CN202010585491.6A CN202010585491A CN111729662A CN 111729662 A CN111729662 A CN 111729662A CN 202010585491 A CN202010585491 A CN 202010585491A CN 111729662 A CN111729662 A CN 111729662A
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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
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
- B01J20/226—Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
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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
- B01J20/28014—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 form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
- C02F2101/103—Arsenic 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
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or 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
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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Abstract
The invention relates to a preparation method and application of an MXene membrane material for in-situ growth of Bi-MOF, and belongs to the technical field of water treatment application and secondary resource recycling. A preparation method of an MXene membrane material with in-situ growth of Bi-MOF comprises the steps of carrying out suction filtration on MXene nanosheet dispersion liquid by a vacuum suction filtration method to enable MXene nanosheets to be attached to a filtering membrane to form an MXene membrane; after the filtration is finished, adding bismuth nitrate solution for secondary vacuum filtration to obtain MXene film containing Bi-O bonds; and (3) placing the MXene film containing the Bi-O bond into a mixed solution of methanol and dimethylformamide, and adding an organic ligand to grow Bi-MOF in situ to obtain the MXene film material of the in-situ grown Bi-MOF. The MXene membrane prepared by the method provided by the invention has the advantages of simple operation process for adsorbing phosphate and heavy metal ions, low operation pressure and environmental friendliness.
Description
Technical Field
The invention relates to a preparation method and application of an MXene membrane material for in-situ growth of Bi-MOF, and belongs to the technical field of water treatment application and secondary resource recycling.
Background
As is known, China has two large fresh water rivers, namely a Yangtze river and a yellow river, which span things, the south and the north of the large river are more numerous fresh water lakes densely distributed in the star, the fresh water resources are extremely rich, but the fresh water resources are seriously damaged along with the rapid development of the national urbanization construction, and heavy metals are one of the most serious pollution sources. According to statistics, half of rivers (more than 10 ten thousand cubic meters) in China are remarkably polluted by about 3/4 lake water areas and 1/2 coastal sea areas, and more, 90% of river basins flowing through cities are polluted by ionic ions such as phosphate radicals, nitrate radicals, heavy metals and the like to different degrees. Nitrogen, phosphorus, etc. are important causes of eutrophication of water, and Total Phosphorus (TP) has been widely used as a standard for eutrophication potential. Phosphorus is generally from agricultural sewage, fertilizer, municipal waste and the like. The form of phosphorus is rather complex, and it is mainly present in the form of organic and inorganic phosphorus in wastewater. Organic phosphorus mainly exists in various organisms and animal excreta, and inorganic phosphorus comprises phosphate, polyphosphate and the like and mainly exists in various phosphate ion forms. The existing sewage dephosphorization methods mainly comprise a chemical precipitation method, an electrolysis method, a microbiological method, a water biological method, a physical adsorption method, a membrane technology treatment method, a soil treatment method and the like. The chemical precipitation method has the problem that some carcinogenic substances exist after reaction, so that the human health is threatened. The electrolysis technology has low current utilization rate, large power consumption and high cost, and can not be widely applied to actual industrial production. The biological treatment method has slow treatment speed and large treatment amount of excess sludge, and is easy to cause secondary pollution. In the physical adsorption method, after adsorbing an organic substance, the adsorbent is difficult to regenerate, and the post-treatment of the spent adsorbent after the reaction is very troublesome, and the secondary pollution is also serious.
Heavy metals are generally toxic or carcinogenic, some of them can show strong toxicity even at low concentration, and what is worse, heavy metals are different from organic pollutants and cannot reduce pollution in a biodegradation mode. In addition, it gradually accumulates in the organism, extending to the highest end of the biological chain, so that heavy metal pollution seriously undermines the ecological balance and human health. Heavy metal pollution is harmful, but is ignored by people because the latent period is long and difficult to find. It was said that water was preferentially acquired in Town by Nippon county in Japan until the 50 th century that this invisible water-contaminated killer went into people's field of vision. China in the industrial development is particularly troubled by heavy metal pollution. Therefore, how to separate heavy metals from water is a very slow task. At present, a plurality of methods for removing heavy metals are available, and the most common methods comprise chemical precipitation, ion exchange, biotechnology, membrane separation, adsorption and the like. In comparison, the membrane separation method is simple and convenient to operate, is green and harmless, and is a method for efficiently treating the water pollution problem.
Disclosure of Invention
In order to solve the problems existing in the process that a powder adsorbent adsorbs phosphate and heavy metal ions thereof, the invention provides an MXene membrane material for in-situ growth of Bi-MOF, which can filter and adsorb phosphate and heavy metal ions thereof in a water body. The technical scheme adopted by the invention is as follows:
a preparation method of an MXene membrane material with in-situ growth of Bi-MOF comprises the steps of carrying out suction filtration on MXene nanosheet dispersion liquid by a vacuum suction filtration method to enable MXene nanosheets to be attached to a filtering membrane to form an MXene membrane; after the filtration is finished, adding bismuth nitrate solution for secondary vacuum filtration to obtain MXene film containing Bi-O bonds; and (3) placing the MXene film containing the Bi-O bond into a mixed solution of methanol and dimethylformamide, and adding an organic ligand to grow Bi-MOF in situ to obtain the MXene film material of the in-situ grown Bi-MOF.
The MXene nanosheet can be prepared by the method disclosed by the prior art. For example: obtained by separation using MAX materials: the MXene dispersion is prepared from MAX phase material mainly comprising Ti3AlC2、Ti2AlN、 Ti4AlN3、Ti3SiC2、Ta4AlC3The separation method is HF corrosion or slow-release HF corrosion preparation generated by an acid deep eutectic solvent (consisting of choline chloride and a hydrogen bond donor).
Preferably, the concentration of the MXene nanosheet dispersion is 0.5-5mg/mL, and the diameter of the MXene nanosheet ranges from 2-5 μm.
Preferably, the vacuum filtration conditions are as follows: carrying out suction filtration operation under the negative pressure of 60-100 Kpa; the filtering membrane is a polyvinylidene fluoride membrane, a polyacrylonitrile membrane or a polyether sulfone membrane with the average pore diameter of 0.25-0.65 mu m.
Preferably, the mass ratio of the bismuth nitrate to the MXene nanosheets is 1: 20-1: 50; the concentration of the bismuth nitrate solution is 10-50 mg/L; the organic ligand is 1,3, 5-benzene tricarboxylic acid, 3, 5-pyridine dicarboxylic acid and 2-amino terephthalic acid; the mass ratio of the organic ligand to the MXene film is 1: 1-5: 1.
further, the organic ligand is preferably 1,3, 5-benzene tricarboxylic acid, and the mass ratio of the bismuth nitrate to the MXene film is 1: 20.
preferably, the volume ratio of methanol to dimethylformamide in the mixed solution of methanol and dimethylformamide is 3: 1-10: 1.
preferably, the MXene film containing the Bi-O bond is placed in a mixed solution of methanol and dimethylformamide, an organic ligand is added, and the reaction is carried out for 24 hours at the temperature of 20-50 ℃ to obtain the MXene film material with the in-situ grown Bi-MOF.
Another object of the invention is to provide an application of the MXene membrane material of the obtained in-situ grown Bi-MOF as a filtering membrane.
The method for adsorbing phosphate radical by using MXene membrane material is a filtration and adsorption method, wherein MXene membrane material of in-situ grown Bi-MOF is used as a filtration membrane, and the phosphate radical is separated by filtration under a certain positive pressure or negative pressure.
The method is a filtration and adsorption method, and the MXene membrane material of Bi-MOF grown in situ is used as a filtration membrane to filter and separate target heavy metal ions under a certain positive pressure or negative pressure.
Further, the heavy metal ion is arsenic oxyanion or arsenic oxyanion.
The invention has the beneficial effects that: the MXene membrane prepared by the method provided by the invention is simple and feasible in phosphate radical and heavy metal ion adsorption, large in adsorption capacity and good in treatment effect; the problems of difficult regeneration of the powder adsorbent and the like are avoided, and other reagents do not need to be additionally added; in addition, the prepared Bi-MOF stably exists in a water body for a long time, can realize the recycling of the membrane, is easy for industrial popularization and has good industrial application prospect.
Drawings
FIG. 1 is a diagram of the process for preparing MXene films containing Bi-MOF according to the example;
FIG. 2 is an MXene membrane containing Bi-MOF prepared in example 1.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
The test methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1
(1) Ti to be purchased3AlC2Putting the powder into hydrofluoric acid to react for 32 hours; then centrifugally separating, washing and drying to obtain Ti3C2The powder material is subjected to ultrasonic treatment for 2 hours to obtain Ti3C2The dispersion of (1); then 2mg/mL of Ti3C2The dispersion was placed in a filter of FIG. 1, and the filtration membrane was a polyvinylidene fluoride membrane having an average pore size of 0.25 μm, and vacuum-filtered at a vacuum degree of 60Kpa to obtain Ti3C2A film; due to the presence of bare Ti atoms, Ti3C2The film contains a large amount of hydrophilic groups, and bismuth nitrate with the concentration of 20mg/L is added50mL of the solution was used to adsorb a large amount of bismuth to Ti3C2On the hydrophilic groups of the membrane; then adding Ti3C2The film was placed in a 50mL tank containing methanol and dimethylformamide in a volume ratio of 1: 3, adding 0.8g of 1,3, 5-benzenetricarboxylic acid serving as a ligand into the mixed solution, and reacting for 3 hours in a reaction kettle at the temperature of 120 ℃ to obtain the MXene film material containing the Bi-MOF.
(2) The MXene film material prepared in the above way is placed in a filter to be used as a filtering membrane, 100mL of phosphate solution containing 20mg/L is subjected to adsorption filtration experiment, the obtained filtrate is sampled, and ion chromatographic analysis shows that the concentration of phosphate in the filtrate obtained after filtration is close to 0mg/L, which shows that the MXene film material can effectively intercept phosphate ions.
Example 2
(1) Weighing 6010.1mg of deep eutectic solvent consisting of choline bromide (3894.0mg and 21.16mmol) and hydrofluoric acid (2116.1mg and 42.31mmol), and adding Ti3SiC260.4mg, stirred at 50 ℃ for 48h, with a stirring rate of 1000 rpm. Washing with deionized water until the pH value is 6, further centrifuging, placing in isopropanol under the protection of argon, performing ultrasonic treatment for 0.5h, performing suction filtration for 0.5h with ethanol, and filtering with a filter membrane of polyethersulfone with an average pore size of 0.25 micron to obtain MXene two-dimensional material; then carrying out ultrasonic treatment for 2h to obtain Ti3C2And (3) dispersing the mixture. Then adding 1mg/mL of Ti3C2The dispersion was placed in a filter shown in FIG. 1, and vacuum-filtered at a vacuum degree of 80Kpa to obtain Ti3C2A film; due to the presence of bare Ti atoms, Ti3C2The film contains a large amount of hydrophilic groups, and 50mL of bismuth nitrate solution with the concentration of 15mg/L is added, so that a large amount of bismuth is adsorbed on Ti3C2On the hydrophilic groups of the membrane; then adding Ti3C2The film was placed in a 50mL tank containing methanol and dimethylformamide in a volume ratio of 1: 3, adding 0.8g of 3, 5-dipicolinic acid serving as a ligand into the mixed solution, and reacting for 5 hours in a reaction kettle at the temperature of 130 ℃ to obtain the MXene film material containing the Bi-MOF.
(2) The MXene film material prepared in the above way is placed in a filter to be used as a filtering membrane, 200mL of arsenic oxyanion solution containing 10mg/L is subjected to an adsorption filtration experiment, the obtained filtrate is sampled, and inductive coupling plasma analysis shows that the concentration of arsenic oxyanions in the filtrate obtained after filtration is 0.1mg/L, which shows that the arsenic oxyanions can be effectively intercepted.
Example 3
(1) 6000.5mg of a deep eutectic solution composed of choline chloride (1353.7mg, 9.70mmol), trifluoromethanesulfonic acid (4365.1mg, 28.09 mmol) and potassium fluoride (281.7mg, 4.85mmol) was weighed, and Ta was added2300.1mg AlC, stirred at 65 ℃ for 72h, with a stirring speed of 2000 rpm. Washing with deionized water, centrifuging to pH 7, ultrasonic treating in isopropanol under the protection of argon for 1 hr, vacuum filtering with ethanol for 1 hr, filtering with polyethersulfone membrane with average pore diameter of 0.25 μm to obtain MXene two-dimensional material, and ultrasonic treating for 2 hr to obtain Ta2C, dispersing liquid; then 3mg/mL of Ta2The dispersion of C was placed in a filter shown in FIG. 1, and vacuum-filtered at a vacuum degree of 60Kpa to obtain Ta2C, a film; due to the presence of bare Ta atoms, so that Ta2The C film contains a large amount of hydrophilic groups, and 50mL of bismuth nitrate solution with the concentration of 20mg/L is added, so that a large amount of bismuth is adsorbed on Ta2C, hydrophilic groups of the film; then adding Ta2And placing the C film in a 50mL reactor prepared by mixing methanol and dimethylformamide according to a volume ratio of 1: 3, adding 0.9g of 2-amino terephthalic acid serving as a ligand into the mixed solution, and reacting for 2 hours in a reaction kettle at 100 ℃ to obtain the MXene film material containing the Bi-MOF.
(2) The MXene film material prepared in the above way is placed in a filter to be used as a filtering membrane, 100mL of arsenic oxyanion solution containing 50mg/L is subjected to an adsorption filtration experiment, the obtained filtrate is sampled, and ion chromatographic analysis shows that the concentration of arsenic oxyanions in the filtrate obtained after filtration is less than 2mg/L, which shows that the arsenic oxyanions can be effectively intercepted.
Claims (9)
1. A preparation method of MXene membrane material for in-situ growth of Bi-MOF is characterized by comprising the following steps: carrying out suction filtration on the MXene nanosheet dispersion liquid by using a vacuum suction filtration method to enable the MXene nanosheets to be attached to the filtering membrane to form an MXene membrane; after the filtration is finished, adding bismuth nitrate solution for secondary vacuum filtration to obtain MXene film containing Bi-O bonds; and (3) placing the MXene film containing the Bi-O bond into a mixed solution of methanol and dimethylformamide, and adding an organic ligand to grow Bi-MOF in situ to obtain the MXene film material of the in-situ grown Bi-MOF.
2. The method of claim 1, wherein: the concentration of the MXene nanosheet dispersion is 0.5-5mg/mL, and the diameter range of the MXene nanosheets is 2-5 μm.
3. The method of claim 1, wherein: the vacuum filtration conditions were as follows: carrying out suction filtration operation under the negative pressure of 60-100 Kpa; the filtering membrane is a polyvinylidene fluoride membrane, a polyacrylonitrile membrane or a polyether sulfone membrane with the average pore diameter of 0.25-0.65 mu m.
4. The method of claim 1, wherein: the mass ratio of the bismuth nitrate to the MXene nanosheets is 1: 20-1: 50; the concentration of the bismuth nitrate solution is 10-50 mg/L; the organic ligand is 1,3, 5-benzene tricarboxylic acid, 3, 5-pyridine dicarboxylic acid and 2-amino terephthalic acid; the mass ratio of the organic ligand to the MXene film is 1: 1-5: 1.
5. the method of claim 1, wherein: the volume ratio of the methanol to the dimethylformamide in the mixed solution of the methanol and the dimethylformamide is 3: 1-10: 1.
6. the method of claim 1, wherein: and (3) placing the MXene film containing the Bi-O bond in a mixed solution of methanol and dimethylformamide, adding an organic ligand, and reacting for 24h at the temperature of 20-50 ℃ to obtain the MXene film material with the in-situ grown Bi-MOF.
7. A method for adsorbing phosphate by using the MXene membrane material prepared by the method of claim 1, which is characterized by comprising the following steps: the method is a filtration and adsorption method, wherein MXene membrane material of in-situ grown Bi-MOF is used as a filtration membrane, and phosphate radical is separated by filtration under a certain positive pressure or negative pressure.
8. A method for adsorbing heavy metal ions by using the MXene membrane material prepared by the method of claim 1, which is characterized by comprising the following steps: the method is a filtering and adsorbing method, wherein MXene membrane material of in-situ grown Bi-MOF is used as a filtering membrane, and the filtering and separating are carried out under certain positive pressure or negative pressure to obtain target heavy metal ions.
9. The method of claim 8, wherein: the heavy metal ions are arsenic oxyanions or arsenic oxyanions.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113839038A (en) * | 2021-08-12 | 2021-12-24 | 山东大学 | MOF-derived Bi @ C nano composite electrode material and preparation method thereof |
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| CN113839038A (en) * | 2021-08-12 | 2021-12-24 | 山东大学 | MOF-derived Bi @ C nano composite electrode material and preparation method thereof |
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Application publication date: 20201002 |