CN112028121B - Preparation method of amorphous molybdenum disulfide nano material based on photocatalytic synthesis - Google Patents
Preparation method of amorphous molybdenum disulfide nano material based on photocatalytic synthesis Download PDFInfo
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 33
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 230000015572 biosynthetic process Effects 0.000 title abstract description 23
- 238000003786 synthesis reaction Methods 0.000 title abstract description 22
- 230000001699 photocatalysis Effects 0.000 title abstract description 9
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 12
- -1 ammonium heptamolybdate heptahydrate Chemical class 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 9
- 235000019253 formic acid Nutrition 0.000 claims description 9
- 239000010453 quartz Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052724 xenon Inorganic materials 0.000 claims description 7
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 6
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001228 spectrum Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 18
- 229910052717 sulfur Inorganic materials 0.000 abstract description 15
- 239000011593 sulfur Substances 0.000 abstract description 15
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 14
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 12
- 239000011733 molybdenum Substances 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 11
- 238000001179 sorption measurement Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 8
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 8
- 229940043267 rhodamine b Drugs 0.000 abstract description 8
- 150000007524 organic acids Chemical class 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 7
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052753 mercury Inorganic materials 0.000 abstract description 6
- 238000005286 illumination Methods 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 230000002194 synthesizing effect Effects 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 229910001385 heavy metal Inorganic materials 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 229910052961 molybdenite Inorganic materials 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000005711 Benzoic acid Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 102000006391 Ion Pumps Human genes 0.000 description 1
- 108010083687 Ion Pumps Proteins 0.000 description 1
- 229910016003 MoS3 Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- TVWWSIKTCILRBF-UHFFFAOYSA-N molybdenum trisulfide Chemical compound S=[Mo](=S)=S TVWWSIKTCILRBF-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000011913 photoredox catalysis Methods 0.000 description 1
- 125000003367 polycyclic group Chemical group 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
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Abstract
The invention discloses a preparation method of an amorphous molybdenum disulfide nano material based on photocatalytic synthesis, belonging to the field of material preparation. The method comprises the following steps: mixing a molybdenum source, an organic acid and a sulfur source to prepare a reaction solution; the reaction solution is synthesized by illumination; the solution is removed, washed thoroughly and dried and centrifuged to obtain the product. The invention has the characteristics of simple synthesis process, low synthesis condition requirement, low energy consumption, low manufacturing cost and the like. The prepared amorphous nano material has extremely strong adsorption capacity on mercury and extremely high removal rate on organic dye rhodamine B.
Description
Technical Field
The invention relates to the field of material preparation, in particular to an amorphous molybdenum disulfide nano material synthesized by utilizing formic acid photocatalysis and a preparation method thereof.
Background
Molybdenum disulfide (MoS)2) The nano material is uniqueThe physical and chemical properties (light, electricity and catalysis) have important application values in various fields of photocatalysis, electrochemical catalysis, electronic devices, photoelectric devices, sensors, environmental pollutant removal and the like, and have the characteristics of large specific surface area, strong adsorption capacity, adjustable band gap, rich edge positions, good chemical stability and the like. Amorphous materials with short and long range disorder can provide larger active surface area and more defects and reaction sites, providing more transport paths and channels for electrons and ions than crystals. However, to date, amorphous MoS2Nanomaterials have not received sufficient attention and their potential applications have not been fully explored. The current methods for preparing amorphous nanomaterials are mainly to introduce low temperature, fast reaction, competitive coordination/adsorption and lattice distortion into the synthesis process to prevent or hinder the transformation of the material from the amorphous to the crystalline state. It should be noted that under ambient conditions, the molybdenum, acid, and sulfur sources cannot be directly mixed to obtain a pure amorphous MoS2. Because the elemental sulfur generated in the reaction process is complexed with sulfur ions in the solution to generate disulfide bonds, a single product, mainly MoS, is difficult to obtainxOr MoS3. Therefore, it is necessary to develop a new synthesis strategy for synthesizing stable and high-yield amorphous MoS at normal temperature and pressure by inhibiting the formation of disulfide bonds by preventing sulfide ions from participating in the reduction reaction2And (3) nano materials.
It is well known that photochemistry can provide a reaction pathway that is difficult to accomplish in classical thermochemical reactions, or shorten the reaction process, making the reaction milder. The photons are used as a 'traceless green reagent' to make the photochemical process more green and sustainable. In recent years, photoredox catalysis has achieved tremendous progress and widespread use in polycyclic addition and functionalization of organic substrates, noble metal catalysts, semiconductor synthesis, carbon dioxide reduction, polymer synthesis, and drug synthesis. To the best of our knowledge, there is currently no photochemical synthesis of MoS2The report of (1). The application of photochemistry in molybdenum disulfide synthesis has great potential for synthesizing a nano material with new appearance and new characteristics.
Chinese patent literature discloses 'a defect-rich 1T-2H mixed phase molybdenum disulfide catalyst and a preparation method and application thereof' (CN 111495393A):
1) respectively adding a sulfur source, a molybdenum source and an organic acid into water, and stirring until the sulfur source, the molybdenum source and the organic acid are dissolved to obtain a first mixture;
2) adding absolute ethyl alcohol into the first mixture to obtain a second mixture;
3) sealing the second mixture in a crystallization kettle containing polytetrafluoroethylene lining for crystallization;
4) and cooling the crystallized reactant to room temperature, and carrying out solid-liquid separation to obtain a solid product, namely the defect-rich 1T-2H mixed phase molybdenum disulfide catalyst.
The sulfur source, molybdenum source and organic acid are sodium sulfide, ammonium molybdate and benzoic acid respectively. The molybdenum disulfide catalyst is crystalline and is not amorphous molybdenum disulfide, and thus cannot provide larger active surface area and reaction sites, and cannot provide more electron and ion transmission paths and channels.
Disclosure of Invention
The invention aims to provide an amorphous molybdenum disulfide nano material based on photocatalytic synthesis, aiming at synthesizing amorphous MoS through photocatalysis2Nano material and makes the nano material have larger active surface area and reaction sites.
The purpose of the invention is realized as follows: an amorphous molybdenum disulfide nanomaterial synthesized based on photocatalytic synthesis of formic acid, the amorphous molybdenum disulfide nanomaterial being prepared by:
step (1): mixing a molybdenum source, an organic acid and a sulfur source in a quartz bottle to prepare a reaction solution;
step (2): the reaction solution is synthesized by illumination;
and (3): the solution is removed, washed thoroughly and dried and centrifuged to obtain the product.
The invention also aims to provide a preparation method of the amorphous molybdenum disulfide nano material.
Yet another object of the present invention is achieved by: 2 ml of 5 mmol ammonium heptamolybdate heptahydrate, 2 ml of fifty percent formic acid and 2 ml of 10 mmol sodium sulfide are added into a quartz bottle with the diameter of 2 cm and the volume of 10 ml, and the quartz bottle is sealed and placed under a 300W full-spectrum xenon lamp for irradiation for 3 minutes; collecting all precipitates, and centrifuging in a centrifuge at a centrifugal speed of 10000 rpm for 10 minutes; then washing the mixture for 3 to 5 times by using deionized water, and then putting the mixture into a vacuum oven to dry the mixture for 3 hours at the temperature of 40 ℃ to obtain a product.
The invention further aims to provide application of the amorphous molybdenum disulfide nano material.
A further object of the invention is achieved by: is used for removing heavy metal ion mercury and organic dye rhodamine B in water.
Compared with the prior art, the invention has the beneficial effects that:
the invention innovatively provides a method for quickly and simply synthesizing amorphous MoS under the environmental condition by using light as energy and a traceless catalyst2A method of preparing a nanomaterial. Firstly, directly mixing a molybdenum source, formic acid and a sulfur source, and then reacting under the illumination of a full-spectrum xenon lamp. Finally, the obtained precipitate is washed for many times and dried in vacuum at normal temperature, and the amorphous nano material with small and uniform particle size can be obtained.
In the synthesis process of the material, the used process is safe, efficient and low in energy consumption (only reaction drying is carried out at normal temperature and normal pressure, and harsh synthesis environments such as high temperature and the like are not involved), the instruments are simple (main instruments are a xenon lamp, a centrifugal machine and a quartz bottle), the synthesis time is only 3 minutes, and the operation is extremely simple.
In a word, the preparation method has the advantages of low preparation cost, simple synthesis process, low synthesis condition requirement and low energy consumption, conforms to the sustainable development concept of environmental protection, and has wider scientific research and use values.
Drawings
FIG. 1a is a schematic diagram of the reaction process and mechanism; FIGS. 1b and 1c are TEM images of the prepared sample; figure 1d is an XRD image of the prepared sample.
Fig. 2 is an SEM image of the prepared product.
Fig. 3 is an XRD image of the prepared product.
FIG. 4 is a Raman image of the product after preparation and a phase change of the structure of the product after increasing the Raman laser energy.
FIG. 5 is a nitrogen adsorption curve of the prepared material.
FIG. 6 is a graph of the adsorption performance of the prepared product at pH1-7 for mercury in water, showing that the adsorption of the synthesized molybdenum disulfide to the heavy metal Hg2+ is not disturbed by acidity in the range of pH 1-7. The synthesized molybdenum disulfide has strong adsorption capacity to Hg2+ in a larger pH range.
Fig. 7 is a maximum adsorption curve of the preparation material for mercury at pH = 6. The balance of ion concentration in the solution reaches 200 mg L-1The curve tends to be smooth when the concentration is about, and the maximum adsorption concentration is 4306 mg g-1。
FIG. 8 shows the preparation of the material for 50 mg g-1And (3) an organic dye rhodamine B removal effect curve. After adsorbing for 30 minutes in a dark environment, illuminating under a 300W full-spectrum xenon lamp, and almost all the organic dye rhodamine B in water is removed after 10 minutes (removal rate)>99.9%)。
Detailed Description
The following technical scheme describes the specific implementation mode of the invention in detail:
the present inventors have found that in the conventional method of directly synthesizing molybdenum disulfide by using a molybdenum source, an acid, and a sulfur source, molybdenum disulfide cannot be produced mainly because sulfur ions in the reaction solution participate in reduction to produce elemental sulfur. The generated elemental sulfur can be complexed with sulfur ions in the solution to generate disulfide bonds, so that a molybdenum polysulfide product is directly synthesized by directly adopting a molybdenum source, an acid and a sulfur source under normal temperature and pressure. Therefore, the research firstly finds out the acid which can generate free radicals in a special synthesis mode, so that the sulfur ions are prevented from participating in reduction, and the molybdenum disulfide can be prepared.
The invention relates to a preparation method of an amorphous molybdenum disulfide nano material based on formic acid photocatalytic synthesis, which comprises the following steps:
step (1): mixing a molybdenum source, an organic acid and a sulfur source in a quartz bottle to prepare a reaction solution;
step (2): the reaction solution is synthesized by illumination;
and (3): the solution is removed, washed thoroughly and dried and centrifuged to obtain the product.
The preparation method of the amorphous molybdenum disulfide nano material comprises the following steps of (1), wherein a molybdenum source is ammonium heptamolybdate heptahydrate, an organic acid is formic acid with fifty percent of volume ratio, a sulfur source is sodium sulfide, and the molar ratio of the sodium sulfide to the ammonium heptamolybdate heptahydrate is 2: 1, the volume ratio of the three is 1: 1: 1.
the preparation method of the amorphous molybdenum disulfide nano material in the step (2) is characterized in that a light source is a 300W full-spectrum xenon lamp, and the irradiation time is 3 minutes.
The preparation method of the amorphous molybdenum disulfide nano material in the step (3) is characterized in that the centrifugal drying conditions are as follows: the centrifugal rotating speed is 9500-10000 rpm, and the centrifugal time is 10 minutes; the washing process is deionized water washing for 3-5 times; the drying needs vacuum drying, the drying temperature is 40 ℃, and the drying time is 3 hours.
The synthesized amorphous molybdenum disulfide nano particles are applied to a reagent for removing heavy metal mercury and an organic dye rhodamine B in water.
The invention innovatively synthesizes amorphous molybdenum disulfide nanoparticles by using photocatalytic formic acid at normal temperature and normal pressure for 3 minutes, and the amorphous molybdenum disulfide nanoparticles are in spherical chain connection and have larger specific surface area. The synthesis process is green and environment-friendly, and the cost is low. And the synthesized amorphous molybdenum disulfide has extremely strong adsorption capacity to mercury and can quickly and efficiently remove the organic dye rhodamine B.
Example 1 (FIGS. 1 to 8 are each a corresponding image or curve of the product of example 1)
2 ml of 5 mmol ammonium heptamolybdate heptahydrate, 2 ml of fifty percent formic acid and 2 ml of 10 mmol sodium sulfide were added to a quartz bottle having a diameter of 2 cm and a volume of 10 ml, and the quartz bottle was sealed and irradiated under a 300W full-spectrum xenon lamp for 3 minutes. All the pellets were collected and centrifuged in a centrifuge at 10000 rpm for 10 minutes. Then washing the mixture for 3 to 5 times by using deionized water, and then putting the mixture into a vacuum oven to dry the mixture for 3 hours at the temperature of 40 ℃.
The amorphous molybdenum disulfide nano material is applied to removing heavy metal ion pumps and organic dye rhodamine B in water. The removal efficiency of rhodamine B is as high as 99%.
Claims (1)
1. A preparation method of an amorphous molybdenum disulfide nano material is characterized in that 2 ml of 5 mmol ammonium heptamolybdate heptahydrate, 2 ml of fifty-percent formic acid by volume and 2 ml of 10 mmol sodium sulfide are added into a quartz bottle, and the quartz bottle is sealed and then placed under a 300W full-spectrum xenon lamp for irradiation for 3 minutes; collecting all precipitates, and centrifuging in a centrifuge at a centrifugal speed of 10000 rpm for 10 minutes; then washing the mixture for 3 to 5 times by using deionized water, and then putting the mixture into a vacuum oven to dry the mixture for 3 hours at the temperature of 40 ℃ to obtain a product.
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