CN109589933B - Magnetic nano composite material UiO-66/Fe3O4Preparation method and application of/GO - Google Patents
Magnetic nano composite material UiO-66/Fe3O4Preparation method and application of/GO Download PDFInfo
- Publication number
- CN109589933B CN109589933B CN201811521852.XA CN201811521852A CN109589933B CN 109589933 B CN109589933 B CN 109589933B CN 201811521852 A CN201811521852 A CN 201811521852A CN 109589933 B CN109589933 B CN 109589933B
- Authority
- CN
- China
- Prior art keywords
- uio
- magnetic
- composite material
- solution
- application
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- 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]
-
- 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
- B01J20/28009—Magnetic properties
-
- 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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- 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
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
-
- 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
- C02F2101/006—Radioactive compounds
Abstract
The invention relates to a magnetic nano composite material UiO-66/Fe3O4A preparation method and application of/GO belong to the technical field of composite materials. UiO-66/Fe is synthesized by one-step synthesis3O4Anchoring the nano-microspheres on a GO sheet layer to obtain UiO-66/Fe3O4a/GO magnetic nanocomposite. The composite material prepared by the method overcomes the defects that graphene sheets are easy to stack and Fe is easy to generate3O4The nano particles are easy to agglomerate, and the nano cavities and Cs thereof+The radius has good compatibility. The adsorbent is used for adsorbing Cs in water+And excellent adsorption performance is shown. UiO-66 modified by magnetic material and GO not only for Cs+Has good adsorbability, and the material is easy to separate due to the magnetism of the material. Therefore, the invention has the characteristics of simple preparation process, good stability, high adsorption efficiency, easy solid-liquid separation, easy recovery, environmental protection and the like.
Description
Technical Field
The invention belongs to the technical field of composite materials, and relates to a magnetic nano composite material UiO-66/Fe3O4Preparation method of/GO and application of material to Cs in aqueous solution+The adsorption removal of (1).
Background
With the increase of global energy demand and the enhancement of environmental protection awareness, carbon-free nuclear power plays an important role in the development of the human society as a key alternative energy of fossil fuels. However, the disposal of radioactive waste in nuclear fission has still limited the development of carbonless nuclear power. Wherein, radioactive cesium (C)137Cs) is a fission-producing radioactive substance, accounting for 6.3% of fission products. It is the major cause of radioactive contamination and is also the most abundant species in nuclear power plant accidents and nuclear waste disposal. Radioactive cesium is a strong gamma radiation source with a long half-life (T)1/230.17 years), biogeochemistry with potassiumThe behavior is similar. It has excellent fluidity and poses serious threats to the environment and human health through continuous flow in the food chain. Therefore, prior to long-term storage of nuclear waste, radioactive ions must be eliminated to reduce the radioactivity below the allowable range. Various processing techniques have been used to remove the radionuclide cesium from aqueous solutions with high adsorption efficiency, simplicity, flexibility and reasonable price. The adsorption process does not use any toxic organic solvent. However, many of these adsorbents are not reproducible and are often associated with environmental hazards. Therefore, efficient and low cost materials should be sought for the selective removal of cesium-containing wastewater.
UiO-66 as a three-dimensional porous zirconium-based MOF, consisting of a 1, 4-phthalic acid linker and a cation Zr6O4(OH)4The node composition has octahedral and tetrahedral cavities, and has received great attention due to its excellent thermal stability, water stability, acid stability and easy synthesis. However, UiO-66 is typically in powder form and is not conducive to separation from solution. Magnetic separation can quickly and easily separate solid materials from liquids. Fe3O4Magnetic nanoparticles have been widely studied due to their low production cost, ease of preparation and large-scale production capability. However, magnetic nanomaterials have magnetic properties and large active surfaces, and the strong interparticle interactions between the magnetic nanoparticles make them difficult to further apply. The immobilization of the magnetic nanoparticles on the substrate is stable Fe3O4Nanoparticles and a feasible method of reducing aggregation. Graphene oxide is an ideal platform for forming new composites because it has hydrophilicity and the availability of hydroxyl, epoxy and carbocyclyl groups, which allow for excellent dispersion in solution. Furthermore, GO may also be used as an adsorbent. Fe3O4The magnetic nanoparticles are anchored on GO. The magnetization of the sorbent matrix facilitates the recovery of the sorbent used and provides a simple and feasible solution to the removal of the target species from the solution. The composite material prepared by the method overcomes the defects that graphene sheets are easy to stack and Fe3O4The nano particles are easy to agglomerate, and the nano cavities and Cs thereof+Radius toolHas good compatibility. The adsorbent is used for adsorbing Cs in water+And excellent adsorption performance is shown. UiO-66 modified by magnetic material and GO not only for Cs+Has good adsorbability, and the material is easy to separate due to the magnetism of the material.
Disclosure of Invention
The invention aims to provide a method which is simple to operate, easy to separate, green and environment-friendly and can be used for adsorbing Cs+The method for preparing the magnetic nanocomposite. The invention synthesizes a magnetic nano composite material UiO-66/Fe3O4/GO with GO as carrier, Fe3O4As core, UiO-66 as shell, UiO-66/Fe3O4The beads are anchored to the GO sheet to give UiO-66/Fe3O4the/GO nano composite material can be applied to Cs in aqueous solution+And (4) removing by adsorption.
Magnetic nano composite material UiO-66/Fe3O4A preparation method of/GO comprises the following steps:
(1) placing graphene oxide in an N, N-dimethylformamide solution, and carrying out ultrasonic treatment for 5-8 hours at the ultrasonic power of 300W to fully dissolve the graphene oxide solid in the N, N-dimethylformamide solution;
(2) after the graphene oxide is fully dissolved, adding ferroferric oxide particles, and carrying out ultrasonic treatment for 10 minutes to obtain a mixed solution;
(3) adding zirconium tetrachloride powder into the mixed solution, carrying out ultrasonic treatment for 30 minutes, and then mechanically stirring for 12 hours at the speed of 200 rpm;
(4) adding terephthalic acid powder after mechanical stirring, and continuing stirring for 30 minutes;
(5) loading the treated mixed solution into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, heating the high-pressure reaction kettle to 120 ℃, and maintaining the reaction for 24 hours;
(6) cooling to room temperature after reaction, filtering, washing the solid with ethanol and deionized water, separating from the solution by magnetic separation, and finally freeze-drying the obtained black solid to obtain the magnetic nano composite material UiO-66/Fe3O4/GO。
The ratio of the ethanol to the deionized water is 1:1, and the washing is carried out for more than 3 times.
The composite material prepared by the invention is used for adsorbing radioactive substances; the radioactive substance is Cs+。
The invention has the advantages that:
(1) the composite material prepared by the method overcomes the defects that graphene sheets are easy to stack and Fe is easy to generate3O4The nano particles are easy to agglomerate, and the nano cavities and Cs thereof+The radius has good compatibility. The adsorbent is made to adsorb Cs in water+Exhibits excellent adsorption performance;
(2) UiO-66 modified by magnetic material and GO, and UiO-66/GO modified by nonmagnetic material and UiO-66/Fe modified by GO3O4Compared with not only to Cs+Has good adsorbability, and the material is easy to separate due to the magnetism of the material.
(3) The invention has the characteristics of simple preparation process, good stability, high adsorption efficiency, easy solid-liquid separation, easy recovery, environmental protection and the like;
(3) the magnetic nano composite material UiO-66/Fe prepared by the invention3O4the/GO takes GO as a carrier, and has the characteristics of good acid and alkali resistance, good thermal stability and easiness in solid-liquid separation.
Drawings
FIG. 1(a) shows UiO-66/Fe obtained in example 23O4Scanning electron micrograph of composite Material, FIG. 1(b) is UiO-66/Fe obtained in example 23O4FIG. 1(c) is a transmission electron micrograph of the composite material, which shows UiO-66/Fe obtained in example 33O4Scanning electron micrograph of/GO composite, FIG. 1(d) is UiO-66/Fe prepared in example 33O4Transmission electron microscopy of the/GO composite.
FIG. 2(a) shows UiO-66/Fe obtained in example 33O4Hysteresis curve diagram of/GO composite material, FIG. 2(b) is UiO-66/Fe prepared in example 33O4Pergo compositeComparison of the effects before and after magnetic separation.
FIG. 3 shows solid UiO-66 material prepared in example 1 and UiO-66/Fe prepared in example 23O4Composite and UiO-66/Fe prepared in example 33O4(ii) use of/GO composites in different Cs+To Cs at initial concentration+Adsorption efficiency curve of (1).
FIG. 4 shows solid UiO-66 material prepared in example 1 and UiO-66/Fe prepared in example 23O4Composite and UiO-66/Fe prepared in example 33O4(GO) composite material for Cs under different adsorption time+Adsorption efficiency curve of (1).
FIG. 5 shows solid UiO-66 material prepared in example 1 and UiO-66/Fe prepared in example 23O4Composite and UiO-66/Fe prepared in example 33O4(GO) composites to Cs at different temperatures+Adsorption efficiency curve of (1).
FIG. 6 shows solid UiO-66 material prepared in example 1 and UiO-66/Fe prepared in example 23O4Composite and UiO-66/Fe prepared in example 33O4(ii) Cvs. Cs of/GO composite under different pH conditions+Adsorption efficiency curve of (1).
Detailed Description
The present invention will be described in detail with reference to the following examples in order to better understand the objects, features and advantages of the present invention. While the invention is described in conjunction with the specific embodiments, it is not intended that the invention be limited to the specific embodiments described. On the contrary, alternatives, modifications and equivalents may be made to the embodiments as may be included within the scope of the invention as defined by the appended claims. The process parameters not specifically mentioned can be carried out according to conventional techniques.
The embodiment of the invention provides a method for adsorbing Cs in an aqueous solution+Magnetic nanocomposite material UiO-66/Fe3O4/GO。
Example 1:
preparation of UiO-66
Dissolving 0.386g of zirconium tetrachloride powder and 0.276g of terephthalic acid powder in N, N-dimethylformamide solution, pouring the solution into a 100mL reaction kettle after a uniform mixed solution is formed, heating the solution at 120 ℃ for 24h, naturally cooling the solution to room temperature, centrifuging the solution, washing the solution with ethanol and deionized water for a plurality of times, and freeze-drying the solution to obtain white powder, namely UiO-66 solid.
Example 2:
magnetic nanocomposite UiO-66/Fe3O4Preparation of
0.1g of ferroferric oxide particles are immersed into 40mL of N, N-dimethylformamide solution and subjected to ultrasonic treatment for 30 minutes to obtain a ferroferric oxide mixed solution. In addition, 0.15g of zirconium tetrachloride powder and 0.1062g of terephthalic acid powder were sequentially added to 30mL of an N, N-dimethylformamide solution and sonicated for 10 minutes to obtain a MOF precursor solution. And pouring the ferroferric oxide mixed solution into the MOF precursor solution and carrying out ultrasonic treatment until the solid particles are uniformly dispersed in the solution. The uniformly mixed solution was poured into a 100mL autoclave, placed in an oven at 80 ℃ for 12 hours, and then left at 100 ℃ for 24 hours. The resulting light brown solid was washed several times with ethanol and deionized water and separated from the solution by magnetic separation. Obtaining purified UiO-66/Fe by freeze-drying3O4Compounding the solid.
Example 3:
magnetic nanocomposite UiO-66/Fe3O4Preparation of/GO
0.03g of graphene oxide is placed in 80mL of N, N-dimethylformamide solution and is subjected to ultrasonic treatment for 5-8 hours to be fully dissolved. And after the graphene oxide is fully dissolved, adding 0.075g of ferroferric oxide particles, and carrying out ultrasonic treatment for 10 minutes. Then, 0.1125g of zirconium tetrachloride powder was added to the above mixed solution to conduct ultrasonic treatment for 30 minutes, followed by mechanical stirring for 12 hours. Finally, 0.0797g of terephthalic acid powder was added thereto, and stirring was continued for 30 minutes. The treated mixed solution is put into a 100mL stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, the high-pressure reaction kettle is heated to 120 ℃, and the reaction is maintained for 24 hoursThen (c) is performed. After cooling to room temperature, filtration was carried out and the solid synthesized was washed several times with ethanol and deionized water and separated from the solution by magnetic separation. Finally, the obtained black solid is frozen and dried to obtain UiO-66/Fe3O4a/GO nanocomposite. The saturation magnetization of the magnetic material is 15.53emu g-1As shown in fig. 2 (a).
Furthermore, as can be seen from FIGS. 1(a) and 1(b), graphene oxide has a lamellar structure with many folds, UiO-66/Fe3O4The nanoparticles are attached to the graphene oxide sheet layer in a spherical shape.
Detection of adsorption Properties
The materials prepared in examples 1, 2 and 3 were applied to Cs+The absorption performance is measured as follows:
50.0mL Cs was adsorbed with 0.01g of adsorbent in a 50mL sealed Erlenmeyer flask+The solution was heated and the temperature and rotation speed were controlled by a water bath shaker to maintain the rotation speed at 200 rpm. Measurement of residual Cs Using atomic absorption Spectrophotometer (nov AA 300)+And (4) concentration. To reduce experimental error, three parallel tests were performed simultaneously in each experiment. Cs adsorbed per unit mass of adsorbent+Can be represented by the formula
And (4) calculating. Wherein C is0And Ce(mg·L-1) Cs at initial and equilibrium respectively+Concentration, m (g) mass of adsorbent, V (L) Cs+Volume of solution. As shown in FIG. 3, the amount of adsorption qeWith initial Cs+Increased in concentration and in initial Cs+The concentration is 80 mg.L-157.29mg g are obtained respectively-1，59.93mg·g-1And 62.07mg g-1The equilibrium capacity of (a). UiO-66/Fe3O4The adsorption capacity of/GO is higher than that of UiO-66 and UiO-66/Fe3O4Because the addition of GO increases the surface area of the material, more active sites and Cs are provided+And (4) reacting. At low concentrations, Cs+Is relatively less competitive than other cations. With Cs+Increase of concentrationLiter, Cs+The competition with other cations increases, enabling them to occupy adsorption sites until saturation. When equilibrium is reached, adsorption and desorption are in dynamic equilibrium, resulting in no further increase in adsorption capacity and possibly even a decrease with increasing concentration.
The variation of the adsorption capacity of the adsorbent for different contact times was investigated. 0.01g of the adsorbent prepared in examples 1, 2 and 3 was weighed at 298K and pH 7, and added to 50mL of an initial concentration of 60 mg. L-1Cs of (A)+In the solution, the solution was separately shaken for different times at 200rpm using a constant temperature shaker. Adsorbent vs. Cs over time+Gradually increases the adsorption amount of (a) and finally gradually becomes saturated by adsorption. The research result is shown in figure 4, the synthesized adsorbent has a fast adsorption rate and an equilibrium time of 2 h.
To investigate the effect of temperature on the adsorption properties of the composites, 0.01g of the adsorbents prepared in examples 1, 2 and 3 were added to 50mL of an initial concentration of 60 mg. L at different temperatures of 298K, 308K, 318K and 328K-1Cs of (A)+In the solution, the pH was controlled at 7, and the solution was shaken for 12 hours at 298K with a constant temperature shaker maintaining the speed at 200 rpm. The results are shown in fig. 5, which shows the endothermic reaction characteristics of the adsorption process and the thermal stability of the adsorbent.
The pH value of the solution is one of the important factors influencing the adsorption performance of the adsorbent. 0.01g of the adsorbent prepared in examples 1, 2 and 3 was weighed out and added to 50mL of an initial concentration of 60 mg. L-1Cs of (A)+In the solution, the pH is adjusted to 4-9 by using 0.1M HCl or NaOH, and the solution is shaken for 12h by adopting a constant temperature shaker to keep the rotating speed at 200rpm and the temperature at 298K. As shown in FIG. 6, the adsorbent UiO-66/Fe3O4Maximum adsorption q of GO at pH 8e。
It should be emphasized that the above-described embodiments are merely examples for clearly illustrating the present invention, but the present invention is not limited to the above-described embodiments. Other variants will be apparent to those skilled in the art on the basis of the foregoing description, and it is not necessary to exemplify all the embodiments herein, but rather obvious variations are contemplated which are within the scope of the invention.
Claims (5)
1. Magnetic nano composite material UiO-66/Fe3O4The application of GO for adsorbing the radioactive substance Cs is characterized in that:
the magnetic nano composite material UiO-66/Fe3O4The preparation method of/GO comprises the following steps:
(1) placing graphene oxide in an N, N-dimethylformamide solution, and carrying out ultrasonic treatment for 5-8 hours to fully dissolve graphene oxide solids in the N, N-dimethylformamide solution;
(2) after the graphene oxide is fully dissolved, adding ferroferric oxide particles, and performing ultrasonic treatment to obtain a mixed solution;
(3) adding zirconium tetrachloride powder into the mixed solution for ultrasonic treatment, and then mechanically stirring;
(4) adding terephthalic acid powder after mechanical stirring, and continuing stirring;
(5) filling the treated mixed solution into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, heating the high-pressure reaction kettle to 120 ℃, and maintaining the reaction for 24 hours;
(6) cooling to room temperature after reaction, filtering, washing the solid with ethanol and deionized water respectively, separating from the solution by magnetic separation, and finally drying the obtained black solid to obtain the magnetic nano composite material UiO-66/Fe3O4/GO。
2. The magnetic nanocomposite UiO-66/Fe of claim 13O4The application of GO for adsorbing the radioactive substance Cs is characterized in that: the ultrasonic power is 300W.
3. The magnetic nanocomposite UiO-66/Fe of claim 13O4The application of GO for adsorbing the radioactive substance Cs is characterized in that: the mechanical stirring speed in the step (3) is 200rpm, and the stirring time is 12 hours.
4. The magnetic nanocomposite UiO-66/Fe of claim 13O4The application of/GO for adsorbing radioactive substances Cs is characterized in that the mass ratio of ethanol to deionized water in the step (6) is 1:1, and washing is carried out for more than 3 times.
5. The magnetic nanocomposite UiO-66/Fe of claim 13O4The application of GO for adsorbing the radioactive substance Cs is characterized in that the drying in the step (6) adopts freeze drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811521852.XA CN109589933B (en) | 2018-12-13 | 2018-12-13 | Magnetic nano composite material UiO-66/Fe3O4Preparation method and application of/GO |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811521852.XA CN109589933B (en) | 2018-12-13 | 2018-12-13 | Magnetic nano composite material UiO-66/Fe3O4Preparation method and application of/GO |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109589933A CN109589933A (en) | 2019-04-09 |
| CN109589933B true CN109589933B (en) | 2020-06-16 |
Family
ID=65960900
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811521852.XA Active CN109589933B (en) | 2018-12-13 | 2018-12-13 | Magnetic nano composite material UiO-66/Fe3O4Preparation method and application of/GO |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109589933B (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110560018A (en) * | 2019-09-09 | 2019-12-13 | 中国科学院城市环境研究所 | synthesis of P2O4 composite UiO-66 material and method for adsorbing and separating indium in liquid crystal panel by using same |
| CN110586052B (en) * | 2019-09-25 | 2021-06-01 | 南开大学 | Preparation and application of magnetic composite porous network adsorption material |
| CN111013544A (en) * | 2019-12-23 | 2020-04-17 | 昆明理工大学 | Preparation method and application of graphene oxide loaded UIO-66 composite material |
| CN112547017A (en) * | 2020-11-19 | 2021-03-26 | 福建师范大学福清分校 | MIL-100(Fe) magnetic nano composite material and preparation method thereof |
| CN112547018A (en) * | 2020-11-19 | 2021-03-26 | 福建师范大学福清分校 | Magnetic nano composite material and preparation method thereof |
| CN113030308B (en) * | 2021-03-02 | 2022-10-28 | 浙江省农业科学院 | Detection method of sulfonamide antibiotics in biogas slurry and sample treatment method thereof |
| CN113030309B (en) * | 2021-03-02 | 2022-12-23 | 浙江工业大学 | Method for detecting nitroimidazole antibiotics in honey and sample treatment method thereof |
| CN113447532B (en) * | 2021-06-25 | 2023-06-30 | 杭州电子科技大学 | Fe (Fe) 3 O 4 Preparation method of air sensor with@UiO-66 structure |
| CN114797782B (en) * | 2021-10-29 | 2023-06-16 | 天津大学 | Magnetic graphene oxide-metal organic framework nanocomposite and preparation method and application thereof |
| CN115463641A (en) * | 2022-08-09 | 2022-12-13 | 国家能源集团科学技术研究院有限公司 | Ternary magnetic composite material and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102836693A (en) * | 2012-09-19 | 2012-12-26 | 清华大学 | Magnetic-nucleus coated type inorganic ion adsorbent used for removing Cs ions in radioactive wastewater, and preparation method of same |
| WO2013106712A1 (en) * | 2012-01-11 | 2013-07-18 | William Marsh Rice University | Composites for carbon dioxide capture |
| CN105233799A (en) * | 2015-06-03 | 2016-01-13 | 西北师范大学 | Magnetic metal-organic framework material with core-shell structure and preparation method therefor |
| CN105344327A (en) * | 2015-11-26 | 2016-02-24 | 中国科学院生态环境研究中心 | Preparation method of MOFs graphene composite material |
| CN107469633A (en) * | 2017-08-17 | 2017-12-15 | 南京工业大学 | It is a kind of to prepare the method with enhancing water flux film |
-
2018
- 2018-12-13 CN CN201811521852.XA patent/CN109589933B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013106712A1 (en) * | 2012-01-11 | 2013-07-18 | William Marsh Rice University | Composites for carbon dioxide capture |
| CN102836693A (en) * | 2012-09-19 | 2012-12-26 | 清华大学 | Magnetic-nucleus coated type inorganic ion adsorbent used for removing Cs ions in radioactive wastewater, and preparation method of same |
| CN105233799A (en) * | 2015-06-03 | 2016-01-13 | 西北师范大学 | Magnetic metal-organic framework material with core-shell structure and preparation method therefor |
| CN105344327A (en) * | 2015-11-26 | 2016-02-24 | 中国科学院生态环境研究中心 | Preparation method of MOFs graphene composite material |
| CN107469633A (en) * | 2017-08-17 | 2017-12-15 | 南京工业大学 | It is a kind of to prepare the method with enhancing water flux film |
Non-Patent Citations (1)
| Title |
|---|
| "UiO-66/GO纳米复合材料的制备及吸附性能";冯胜等，;《精细化工》;20181130;第35卷(第11期);第1942页摘要、第1943页1.2复合材料的制备 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109589933A (en) | 2019-04-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109589933B (en) | Magnetic nano composite material UiO-66/Fe3O4Preparation method and application of/GO | |
| Han et al. | Hydrothermal carbon superstructures enriched with carboxyl groups for highly efficient uranium removal | |
| Yu et al. | Sorption of radionuclides from aqueous systems onto graphene oxide-based materials: a review | |
| Huo et al. | Selective adsorption of cesium (I) from water by Prussian blue analogues anchored on 3D reduced graphene oxide aerogel | |
| Zhu et al. | Adsorption removal of congo red onto magnetic cellulose/Fe3O4/activated carbon composite: Equilibrium, kinetic and thermodynamic studies | |
| Zhang et al. | Hierarchically porous bismuth oxide/layered double hydroxide composites: preparation, characterization and iodine adsorption | |
| Zhang et al. | Fluoride adsorption from aqueous solution by magnetic core-shell Fe3O4@ alginate-La particles fabricated via electro-coextrusion | |
| Sun et al. | Direct synthesis of bacteria-derived carbonaceous nanofibers as a highly efficient material for radionuclides elimination | |
| Dong et al. | Construction of oxidized millimeter-sized hierarchically porous carbon spheres for U (VI) adsorption | |
| Yang et al. | Characteristics of cesium ion sorption from aqueous solution on bentonite-and carbon nanotube-based composites | |
| Wei et al. | Magnetic separation of uranium by CoFe2O4 hollow spheres | |
| Lu et al. | Spectroscopic and modeling investigation of efficient removal of U (VI) on a novel magnesium silicate/diatomite | |
| Arica et al. | Polyaniline coated magnetic carboxymethylcellulose beads for selective removal of uranium ions from aqueous solution | |
| Li et al. | Enrich and seal radionuclides in magnetic agarose microspheres | |
| Zhao et al. | Reduced graphene oxide/ZIF-67 aerogel composite material for uranium adsorption in aqueous solutions | |
| Li et al. | Fabrication of in situ ZIF-67 grown on alginate hydrogels and its application for enhancing Cu (II) adsorption from aqueous solutions | |
| Cheng et al. | Fabrication of 3D macroscopic graphene oxide composites supported by montmorillonite for efficient U (VI) wastewater purification | |
| Bi et al. | Growth of a mesoporous Zr-MOF on functionalized graphene oxide as an efficient adsorbent for recovering uranium (VI) from wastewater | |
| Sun et al. | Adsorption behavior and mechanism of U (VI) onto phytic Acid-modified Biochar/MoS2 heterojunction materials | |
| Wang et al. | Natural porous wood decorated with ZIF-8 for high efficient iodine capture | |
| CN105854744B (en) | A kind of magnetic nanoparticle/SiO2Aeroge and preparation method thereof and the method for handling high activity liquid waste | |
| Zhuang et al. | Selective and effective adsorption of cesium ions by metal hexacyanoferrates (MHCF, M= Cu, Co, Ni) modified chitosan fibrous biosorbent | |
| Li et al. | Magnetic chitosan microspheres: An efficient and recyclable adsorbent for the removal of iodide from simulated nuclear wastewater | |
| Wei et al. | Interaction of U (VI) with amine-modified peanut shell studied by macroscopic and microscopic spectroscopy analysis | |
| Wang et al. | Scalable Fe@ FeO core-shell nanoparticle-embedded porous wood for high-efficiency uranium (VI) adsorption |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |