CN115138330A - Synthetic Fe 3 O 4 Method for preparing @ MCM-56 magnetic nano composite material - Google Patents
Synthetic Fe 3 O 4 Method for preparing @ MCM-56 magnetic nano composite material Download PDFInfo
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- CN115138330A CN115138330A CN202210720044.6A CN202210720044A CN115138330A CN 115138330 A CN115138330 A CN 115138330A CN 202210720044 A CN202210720044 A CN 202210720044A CN 115138330 A CN115138330 A CN 115138330A
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- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 20
- 239000000463 material Substances 0.000 title description 11
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000002808 molecular sieve Substances 0.000 claims abstract description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 24
- 239000002131 composite material Substances 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000003755 preservative agent Substances 0.000 claims description 3
- 230000002335 preservative effect Effects 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 241000764238 Isis Species 0.000 claims 1
- 238000003756 stirring Methods 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract description 2
- 238000007598 dipping method Methods 0.000 abstract 1
- 229910000859 α-Fe Inorganic materials 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 21
- 238000001179 sorption measurement Methods 0.000 description 19
- 239000011148 porous material Substances 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- AUHZEENZYGFFBQ-UHFFFAOYSA-N 1,3,5-trimethylbenzene Chemical compound CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical group O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
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- 229910017135 Fe—O Inorganic materials 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
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- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
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- 230000007423 decrease Effects 0.000 description 1
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- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
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- 239000002245 particle Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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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
- B01J20/06—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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
- B01J20/183—Physical conditioning without chemical treatment, e.g. drying, granulating, coating, irradiation
-
- 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
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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
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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Abstract
The invention discloses a method for synthesizing Fe 3 O 4 A method of @ MCM-56 magnetic nanocomposite, the method being a dipping method: mixing ferrite Fe 3 O 4 Combined with mesoporous molecular sieve MCM-56, and subjected to ultrasonic, stirring and water bath heating to obtain Fe with a shell-core structure 3 O 4 @ MCM-56 magnetic nanocomposite. The method has the advantages of simple operation, mild conditions and less sample consumption, and greatly reduces the manufacturing cost.
Description
Technical Field
The invention relates to the technical field of synthesis of magnetic porous materials, in particular to a method for synthesizing Fe 3 O 4 A process for the manufacture of a @ MCM-566 magnetic nanocomposite.
Background
The molecular sieve is aluminosilicate, is a common molecular sieve in nature called natural zeolite, has wide application in many fields, can be used for preparing drying agents, catalysts, ion exchangers and the like, is also an excellent adsorbent for coal gas dehydration, and is increasingly emphasized on waste gas purification. The MCM-56 molecular sieve is a honeycomb-like layered structure molecular sieve and consists of an extremely thin single-layer MWW structure, has strong hydrothermal stability and special acid center distribution, can be used as a novel catalytic material, and can be used as an adsorbent due to strong adsorption capacity on molecules. MCM-56 molecular sieves have pore sizes similar to those of molecules and are honeycomb-like in shape, and can select molecules. Compared with MCM-22 and MCM-49 molecular sieves, the adsorption capacity of the MCM-56 molecular sieve to 1,3,5-trimethylbenzene is more than 4 times that of the two molecular sieves after roasting. In the aspects of adsorbing heavy metal ions, organic pollutants, antibiotics and the like, the MCM-56 molecular sieve shows extremely strong adsorption capacity due to large specific surface area and many cavities.
The novel magnetic molecular sieve adsorbent material is a novel magnetic material with a porous structure and simple preparation, and has the characteristics of good micro-nano structure, strong adsorption performance, simple and quick magnetic separation and the like, so that the novel magnetic molecular sieve adsorbent material can play an important role in the fields of gas emission treatment, environmental protection and the like. And Fe 3 O 4 The nano particles are typical magnetic nano materials with the advantages of low toxicity, simple preparation process, low cost, superparamagnetism, small particle size, large specific surface area, easy recovery and the like, are commonly used as the inner cores of shell-core composite materials, and are widely applied to various fields.
In recent years, many researches on Fe3O4 and other nano composite materials exist, but no researchers at present research on the coating of the MCM-56 molecular sieve on the Fe3O4 nano particles.
Disclosure of Invention
The invention aims to provide a synthetic Fe aiming at overcoming the defects of the prior art 3 O 4 A process for the manufacture of a magnetic nanocomposite material of @ MCM-56. The method has the advantages of simple operation, mild conditions, less sample consumption and low manufacturing cost.
The technical scheme for realizing the purpose of the invention is as follows:
synthetic Fe 3 O 4 A process for the manufacture of a @ MCM-56 magnetic nanocomposite, comprising the steps of:
s1, respectively weighing 0.024g-0.06g of ferroferric oxide, 0.12g-0.15g of MCM-56 molecular sieve and 100g of deionized water;
s2, pouring weighed ferroferric oxide and MCM-56 molecular sieve into a beaker filled with deionized water to prepare a mixed solution, then placing the beaker into an ultrasonic cleaner with the water bath temperature of 50 ℃ for ultrasonic treatment for 3-5 h, meanwhile, keeping the liquid in the beaker in a stirred state all the time, and sealing the opening of the beaker filled with the mixed solution by using a preservative film;
s3, placing the beaker filled with the mixed solution into a constant-temperature drying box, and drying for 10 hours at the temperature of 90 ℃;
s4, pouring the dried experimental sample into an agate pot, and uniformly grinding to finally obtain the composite material Fe 3 O 4 @MCM-56。
The steps S1 to S4 can be repeated, and the temperature of the water bath is changed;
or repeating the steps from S1 to S4, and changing the mass ratio of the ferroferric oxide to the MCM-56 molecular sieve.
When the mass of the ferroferric oxide in the step S1 is 0.024g, the ultrasonic time in the step S2 is 5h.
When the mass of the ferroferric oxide in the step S1 is 0.0375g and the mass of the MCM-56 molecular sieve is 0.15g, the ultrasonic time in the step S2 is 5 hours.
When the mass of the ferroferric oxide in the step S1 is 0.025g and the mass of the MCM-56 molecular sieve is 0.15g, the ultrasonic time in the step S2 is 5 hours.
The technical proposal adopts an immersion method to directly react Fe 3 O 4 And the synthesized MCM-56 molecular sieve is subjected to ultrasonic stirring to ensure that Fe is generated 3 O 4 Permeates into MCM-56 molecular sieve to form magnetic nano composite material Fe with practical value and core/shell structure 3 O 4 @MCM-56。
The method has the advantages of simple operation, mild conditions and less sample consumption, and greatly reduces the manufacturing cost.
Drawings
The XRD pattern of the MCM-56 molecular sieve in the example of FIG. 1;
fe in the example of FIG. 2 3 O 4 An XRD pattern of (a);
FIG. 3 example Fe composite prepared in example 2 3 O 4 The XRD pattern of @ MCM-56;
FIG. 4 example Fe composite prepared in example 2 3 O 4 The nitrogen adsorption and desorption isotherm and the pore size distribution map of the @ MCM-56;
FIG. 5 shows the nitrogen adsorption-desorption isotherm and pore size distribution of the MCM-56 molecular sieve prepared in example 2;
FIG. 6 shows MCM-56, fe in example 3 O 4 With Fe 3 O 4 A benzene adsorption data plot for a @ MCM-56 magnetic nanocomposite;
FIG. 7 is Fe composite material prepared in example 3 O 4 TEM image of @ MCM-56.
Detailed Description
The invention will be further illustrated by the following figures and examples, but is not limited thereto.
Example (b):
example 1:
synthetic Fe 3 O 4 A method of @ MCM-566 magnetic nanocomposite, comprising the steps of:
s1, respectively weighing 0.04g of ferroferric oxide, 0.12g of MCM-56 molecular sieve and 100g of deionized water;
s2, pouring weighed ferroferric oxide and MCM-56 molecular sieve into a beaker filled with deionized water to prepare a mixed solution, then placing the beaker into an ultrasonic cleaner with the water bath temperature of 50 ℃ for ultrasonic treatment for 3 hours, simultaneously keeping the liquid in the beaker in a stirred state all the time, and sealing the opening of the beaker filled with the mixed solution by using a preservative film;
s3, placing the beaker filled with the mixed solution into a constant-temperature drying box, and drying for 10 hours at the temperature of 90 ℃;
s4, pouring the dried experimental sample into an agate pot, and uniformly grinding to finally obtain the composite material Fe 3 O 4 @MCM-56。
Example 2:
in this example, the mass of ferroferric oxide in step S1 is 0.024g, and the ultrasonic time in step S2 is 5 hours, as in example 1.
Example 3:
in this example, the mass of ferroferric oxide in step S1 was 0.0375g, the mass of MCM-56 molecular sieve was 0.15g, and the ultrasonic time in step S2 was 5 hours, as in example 1.
Example 4:
in this example, the mass of ferroferric oxide in step S1 is 0.025g, the mass of the MCM-56 molecular sieve is 0.15g, and the ultrasonic time in step S2 is 5 hours, as in example 1.
Table 1 shows Fe prepared in examples 1 to 4 3 O 4 BET structure parameters of a @ MCM-56 magnetic nanocomposite:
table 1: BET structural parameters of the samples obtained in 4 examples
Table 2: MCM-56 with Fe 3 O 4 Benzene adsorption capacity of @ MCM-56 magnetic nanocomposite
For MCM-56 molecular sieve and Fe 3 O 4 And the composite Fe prepared in the examples 3 O 4 Characterization analysis was performed with @ MCM-56:
as shown in figure 1, in the reagent prepared by the MCM-56 molecular sieve, the raw material silicon-aluminum ratio (SiO 2/AlO 3) is 30, the composite template agent is HMI/AN, the reagent is prepared under the condition of dynamic crystallization at the crystallization temperature of 145 ℃ for 9 days, the sample is respectively obvious broad peaks at 2 theta = 8-11 degrees and 22.5 degrees, diffraction peaks of 101 and 102 are overlapped and stably decline at the temperature of 26-29 degrees, and a longer tailing peak is presented;
as shown in FIG. 2, fe 3 O 4 Typical characteristic diffraction peaks 2 θ =30.12 °,35.51 °,43.18 °,53.49 °,57.07 °,62.70 °, and 74.1 °;
as shown in FIG. 3, specifically, FIG. 3 shows that the sample is subjected to ultrasonic treatment and stirring for 5h, the water bath temperature is 50 ℃, and Fe 3 O 4 An XRD pattern of the product generated under the condition that the mass percentage is 16.7 percent shows characteristic diffraction peaks of the MCM-56 molecular sieve in 2 theta =7.18 degrees, 14.73 degrees, 20.08 degrees, 22.46 degrees, 25.20 degrees and 26.23 degrees, which shows that the crystal structure of the MCM-56 molecular sieve is not damaged and the sample still contains pure-phase MCM-56 molecular sieve in the process of preparing the magnetic nanocomposite by using the MCM-56 molecular sieve, and in addition, fe appears in 2 theta =30.12 degrees, 35.51 degrees and 43.18 degrees 3 O 4 Typical characteristic peaks of (A), indicating that the resulting product still contains Fe 3 O 4 . The final result of the XRD pattern shows that the prepared experimental sample contains MCM-56 molecular sieve and Fe 3 O 4 ；
As shown in FIG. 4, FIG. 4 shows that the sample is subjected to ultrasonic treatment and stirring for 5h, the water bath temperature is 50 ℃, and Fe 3 O 4 FT-IR chart of the product produced at 16.7% by mass, from which it was observed that the mass fraction was 3455cm -1 To 3464cm -1 An absorption peak is generated because of the super-strong polarity of the hydroxyl, so that the occurrence of hydrogen bonds is easily caused, and the absorption peak corresponds to the stretching vibration peak of the hydroxyl; at wave number 2381cm -1 In the vicinity, the transmittance fluctuates due to CO in the air while the potassium bromide is used for tableting 2 Caused by penetration into the sample; 1637cm due to residual or attached water in the sample -1 The vicinity thereof exhibited a bending vibration peak of the hydroxyl group. It is shown in the literature that the thickness of the coating is at 1092cm -1 And 804cm -1 The absorption peak is caused by the asymmetric and symmetric expansion and contraction of T-O tetrahedron in the material. At 593cm -1 And 570cm -1 The composite material has a framework double-ring vibration peak of the MCM-56 molecular sieve, and is known to be 400-900 cm according to related documents -1 The infrared absorption peak is used for representing the molecular with microporous MWW structureOne of the characteristics of the sieve, in combination with the earlier X-ray diffraction analysis of the experimental sample, further demonstrated that the composite material contains a pure phase MCM-56 molecular sieve, as can be seen in FIG. 4, 590cm -1 A weak peak is nearby. FIG. 7 is the isotherm and pore size distribution of the product produced by subjecting a sample to ultrasound treatment at a water bath temperature of 50 ℃ and a Fe3O4 mass ratio of 16.7%, wherein a heating purge treatment at a purge temperature of 200 ℃ for 3 hours is required before nitrogen adsorption-desorption analysis in order to remove impurities such as water vapor in the sample, as shown in FIG. 7, the isotherm adsorption and desorption curves of the sample are both biased and have a significant hysteresis loop, and in a low relative pressure region, the inflection point is relatively gentle and the adsorption curve tends to rise gently, which indicates that N is a gentle curve 2 The molecules generally formed a monolayer dispersion in the interior channels of the experimental sample, with a smaller slope of the curve for the middle region, indicating N 2 The molecules form multi-layer dispersion in the inner pore canal of the experimental sample, and at the position of P/P0= 0.8-1.0, the sample pair N 2 The adsorption amount of (a) rapidly increases because N2 shows capillary coagulation in the inner pore and the outer surface of the sample, and the hysteresis loop represents capillary coagulation in the mesopores, and further, as can be seen from the pore volume and pore diameter analysis chart of the experimental sample, fe prepared 3 O 4 The pore diameter distribution of the @ MCM-56 magnetic nano composite material is concentrated between 2 and 3nm and just corresponds to Fe 3 O 4 The absorption peak of Fe-O is enough to indicate that the experimental sample contains Fe 3 O 4 ；
As shown in FIG. 5, FIG. 5 shows that Fe is obtained when the water bath temperature of the sample is 50 ℃ and the ultrasonic and stirring time is 3h, 5h and 5h respectively 3 O 4 TEM image of the products formed under the conditions of 14.29%, 16.67%, 20% and 25% in mass ratio, respectively, as can be seen from FIG. 5, in which the black part is Fe 3 O 4 The peripheral light-colored area is partially MCM-56 molecular sieve, and obviously the MCM-56 molecular sieve successfully coats Fe serving as a kernel 3 O 4 Nanoparticles to Fe 3 O 4 @ MCM-56 magnetic nanocomposite;
as shown in FIG. 6, FIG. 6 shows that the sample is subjected to ultrasonic treatment and stirring for 5 hours, the water bath temperature is 50 ℃, and Fe 3 O 4 The benzene adsorption data of the samples prepared under the conditions that the mass ratio of the benzene adsorption data to the MCM-56 molecular sieve is 0%, 16.7%, 20%, 25% and 100%, respectively, can be seen from the graph, and after the experimental sample is prepared by the impregnation method, when Fe is used 3 O 4 When the mass ratio of the Fe-B-C mixed material to the MCM-56 molecular sieve is 16.7 percent 3 O 4 The MCM-56 composite material has the strongest benzene adsorption capacity, the adsorption capacity reaches 190.585mg/g, and the adsorption capacity is 6.73% higher than that of an original molecular sieve, and the reason for causing the adsorption capacity of an experimental sample to rise is deduced as follows: after the ferroferric oxide enters the MCM-56 molecular sieve, the ferroferric oxide and the MCM-56 molecular sieve form a certain special physical structure, the adsorption capacity of the prepared experimental sample on benzene is promoted, and then the adsorption capacity is increased along with Fe 3 O 4 Compared with the increase of the mass ratio of the MCM-56 molecular sieve, the adsorption quantity of the experimental sample to the benzene is reduced to different degrees.
Claims (4)
1. Synthetic Fe 3 O 4 A process for the manufacture of a @ MCM-566 magnetic nanocomposite, characterized in that it comprises the steps of:
s1, respectively weighing 0.024g-0.06g of ferroferric oxide, 0.12g-0.15g of MCM-56 molecular sieve and 100g of deionized water;
s2, pouring weighed ferroferric oxide and MCM-56 molecular sieve into a beaker filled with deionized water to prepare a mixed solution, then placing the beaker into an ultrasonic cleaner with the water bath temperature of 50 ℃ for ultrasonic treatment for 3-5 h, meanwhile, keeping the liquid in the beaker in a stirred state all the time, and sealing the opening of the beaker filled with the mixed solution by using a preservative film;
s3, placing the beaker filled with the mixed solution in a constant-temperature drying box, and drying for 10 hours at the temperature of 90 ℃;
s4, pouring the dried experimental sample into an agate pot, and uniformly grinding to finally obtain the composite material Fe 3 O 4 @MCM-56。
2. Synthetic Fe according to claim 1 3 O 4 A method of @ MCM-566 magnetic nanocomposite, characterized in that when the mass of ferroferric oxide in step S1 is 0.024g, the ultrasonic time in step S2 isIs 5h.
3. Synthetic Fe according to claim 1 3 O 4 The method of the @ MCM-566 magnetic nanocomposite is characterized in that when the mass of the ferroferric oxide in the step S1 is 0.0375g and the mass of the MCM-56 molecular sieve is 0.15g, the ultrasonic time in the step S2 is 5 hours.
4. Synthetic Fe according to claim 1 3 O 4 The method of the @ MCM-566 magnetic nanocomposite is characterized in that when the mass of the ferroferric oxide in the step S1 is 0.025g and the mass of the MCM-56 molecular sieve is 0.15g, the ultrasonic time in the step S2 is 5 hours.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103551094A (en) * | 2013-11-22 | 2014-02-05 | 齐齐哈尔大学 | Preparation method of core-shell structured Fe3O4@MCM-41 magnetic nano material |
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