CN115318310A - Preparation of C-doped MoS 2 @TiO 2 Method for preparing aerogel catalyst - Google Patents
Preparation of C-doped MoS 2 @TiO 2 Method for preparing aerogel catalyst Download PDFInfo
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- CN115318310A CN115318310A CN202210844445.2A CN202210844445A CN115318310A CN 115318310 A CN115318310 A CN 115318310A CN 202210844445 A CN202210844445 A CN 202210844445A CN 115318310 A CN115318310 A CN 115318310A
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- 239000004964 aerogel Substances 0.000 title claims abstract description 31
- 239000003054 catalyst Substances 0.000 title claims abstract description 29
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- 238000002360 preparation method Methods 0.000 title claims description 7
- 101100069231 Caenorhabditis elegans gkow-1 gene Proteins 0.000 title description 2
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- 239000002028 Biomass Substances 0.000 claims abstract description 10
- 238000007710 freezing Methods 0.000 claims abstract description 10
- 230000008014 freezing Effects 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 8
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- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 3
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 27
- ZKKLPDLKUGTPME-UHFFFAOYSA-N diazanium;bis(sulfanylidene)molybdenum;sulfanide Chemical compound [NH4+].[NH4+].[SH-].[SH-].S=[Mo]=S ZKKLPDLKUGTPME-UHFFFAOYSA-N 0.000 claims description 8
- 150000003384 small molecules Chemical class 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 4
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 claims description 3
- 229920002873 Polyethylenimine Polymers 0.000 claims description 3
- 229920002125 Sokalan® Polymers 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 229940072056 alginate Drugs 0.000 claims description 3
- 229920000615 alginic acid Polymers 0.000 claims description 3
- 235000010443 alginic acid Nutrition 0.000 claims description 3
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 3
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 3
- 239000011609 ammonium molybdate Substances 0.000 claims description 3
- 229940010552 ammonium molybdate Drugs 0.000 claims description 3
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 3
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 3
- 239000004584 polyacrylic acid Substances 0.000 claims description 3
- 235000015393 sodium molybdate Nutrition 0.000 claims description 3
- 239000011684 sodium molybdate Substances 0.000 claims description 3
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 3
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 3
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 3
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 3
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- 238000010438 heat treatment Methods 0.000 description 8
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
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- 231100000719 pollutant Toxicity 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical group [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
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Abstract
The present disclosure discloses a method for preparing C-doped MoS 2 @TiO 2 A method of making an aerogel catalyst, comprising the steps of: dissolving natural polysaccharide or micromolecular polymer of biomass in deionized water, and adding MoS 2 Precursor and TiO 2 Stirring the precursor at room temperature to obtain a viscous mixture; freezing and drying the viscous mixture to obtain light gel; calcining the light gel to obtain the C-doped MoS 2 @TiO 2 An aerogel catalyst.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a method for preparing C-doped MoS 2 @TiO 2 A method of preparing an aerogel catalyst.
Background
Along with the rapid development of national socioeconomic, volatile Organic Compounds (VOC) with unorganized emission generated by various large-scale chemical engineering projects s ) Nitrogen oxides, sulfur dioxide, ammonia and the like make the atmospheric environmental pollution problem increasingly severe, and the efficient prevention and control of atmospheric pollutants are of great importance. The current mainstream technology improves the condition of chemical waste gas pollution to a great extent, but has the defects of high treatment cost, short service life of equipment and catalyst, long catalyst regeneration period, secondary pollution and the like. Different from the traditional chemical waste gas treatment technology, the photocatalytic oxidation technology is simple and convenient to operate, green, economical, practical and efficient, but the removal efficiency of the high-concentration (ppm level) VOCs in industrial flue gas is still very limited. In recent years, photocatalytic O 3 、H 2 O 2 And PMS has been studied extensively in water treatment, as opposed to O 2 Or H 2 The efficiency of O as a free radical generating source in the traditional photocatalysis technology for degrading pollutants in water is obviously improved. Is prepared from O 3 、H 2 O 2 And PMS introduces photocatalysis and oxidation VOCs for treatment, and has the potential of treating high-concentration VOCs. The key problem of the photocatalytic oxidation system is the development of high-performance catalyst.
Conventional TiO 2 Semiconductor photocatalysts have two main obstacles, namely weak performance in the photocatalysis process of industrial scale application, low photocatalytic activity due to the limitation of optical utilization rate by wide band gap (3.2 eV), and the aim of exerting TiO 2 The light absorption and utilization activity of (2) are frequently utilized by researchers to dope TiO with C, N and the like 2 Modification, C doping will modify TiO 2 Light absorption property of (2) and TiO 2 Electrons on the conducting stripCan be transferred to the C layer to promote electron-hole separation. Molybdenum disulfide (MoS) 2 ) Is a typical layered compound in which a molybdenum atom is sandwiched between two hexagonal close-packed S atoms by weak van der Waals' force, has a narrow band gap (1.9 eV), is good in chemical stability, large in specific surface area, strong in oxidation property, non-toxic, and it can also be used as TiO 2 Good cocatalyst of nano particles. And MoS 2 And TiO 2 2 In contrast, tiO 2 @MoS 2 Is one of the excellent photocatalysts.
However, the traditional catalysts in powder form have disadvantages in industrial applications: for example, they are easily blown away in air, are difficult to recover, and are harmful to the environment.
Disclosure of Invention
In view of the deficiencies in the prior art, it is an object of the present disclosure to provide a method for preparing C-doped MoS 2 @TiO 2 The aerogel catalyst prepared by the method has the characteristics of stable structure and easy recovery.
In order to achieve the above purpose, the present disclosure provides the following technical solutions:
preparation of C-doped MoS 2 @TiO 2 A method of making an aerogel catalyst, comprising the steps of:
s100: dissolving biomass natural polysaccharide or micromolecular polymer in deionized water, and adding MoS 2 Precursor and TiO 2 Stirring the precursor at room temperature to obtain a viscous mixture;
s200: freezing and drying the viscous mixture to obtain light gel;
s300: calcining the light gel to obtain C-doped MoS 2 @TiO 2 An aerogel catalyst.
Preferably, in step S100, the biomass natural polysaccharide or small molecule polymer has a mass of 0.05-0.2g.
Preferably, the biomass natural polysaccharide comprises carboxymethyl cellulose and alginate.
Preferably, the small molecule polymer comprises polyacrylic acid and polyethyleneimine.
Preferably, the MoS 2 The precursor comprises any one of the following components: ammonium tetrathiomolybdate, a mixture of ammonium molybdate and thiourea, and a mixture of sodium molybdate and thioacetamide.
Preferably, the TiO is 2 The precursor comprises any one of the following components: tetrabutyl titanate, isopropyl titanate, titanium tetrachloride and titanium sulfate.
Preferably, in step S200, the freezing time of the viscous mixture is 5-30min.
Preferably, in step S300, the calcination temperature of the light gel is 150-900 ℃.
Compared with the prior art, the beneficial effect that this disclosure brought does:
1. in the present disclosure, the biomass natural polysaccharide or small molecule polymer serves as both a carbon source and a TiO source 2 The modified ammonium thiomolybdate is used as a template for connecting ammonium thiomolybdate to construct a net structure, and the three-dimensional C-doped MoS is synthesized through a simple self-assembly process design 2 @TiO 2 The aerogel catalyst has larger specific surface area and increases the exposable catalytic active sites;
2. the prepared aerogel catalyst has a layered structure formed by mutually connecting aerogels, is stable and can be recycled, and shows potential application value in the field of wide air purification.
Drawings
FIG. 1 is a schematic diagram of a method for preparing C-doped MoS according to an embodiment of the present disclosure 2 @TiO 2 A flow diagram of a method of aerogel catalysis;
FIG. 2 is a C-doped MoS provided by an embodiment of the present disclosure 2 @TiO 2 An aerogel XRD representation diagram;
FIG. 3 is a C-doped MoS provided by an embodiment of the disclosure 2 @TiO 2 Optical diagram of aerogel before calcination;
FIG. 4 shows a C-doped MoS structure provided by an embodiment of the disclosure 2 @TiO 2 Scanning electron microscope image of aerogel.
Detailed Description
Specific embodiments of the present disclosure will be described in detail below with reference to fig. 1 to 4. While specific embodiments of the disclosure are shown in the drawings, it should be understood that the disclosure can be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
It should be noted that certain terms are used throughout the description and claims to refer to particular components. As one skilled in the art will appreciate, various names may be used to refer to a component. This specification and claims do not intend to distinguish between components that differ in name but not function. In the following description and in the claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. The description which follows is a preferred embodiment of the disclosure, but is made for the purpose of illustrating the general principles of the disclosure and not for the purpose of limiting the scope of the disclosure. The scope of the present disclosure is to be determined by the terms of the appended claims.
For the purpose of facilitating an understanding of the embodiments of the present disclosure, the following detailed description is to be construed in conjunction with the accompanying drawings, and the various drawings are not intended to limit the embodiments of the present disclosure.
In one embodiment, as shown in fig. 1, the present disclosure provides a method of preparing C-doped MoS 2 @TiO 2 A method of aerogel catalyst comprising the steps of:
s100: dissolving biomass natural polysaccharide or micromolecular polymer in deionized water, and adding MoS 2 Precursor and TiO 2 Stirring the precursor at room temperature to obtain a mixture;
s200: freezing and drying the mixture to obtain light gel;
s300: calcining the light gel to obtain C-doped MoS 2 @TiO 2 An aerogel catalyst.
In the embodiment, natural biomass polysaccharide or micromolecular polymer is selected as the material for preparing C-doped MoS 2 @TiO 2 Raw material of aerogel catalyst, which can be used as carbon source to TiO 2 Modified and can be used as a template for connecting ammonium thiomolybdate to construct a net structure, so that the finally prepared C-doped MoS 2 @TiO 2 The aerogel catalyst has larger specific surface area, and increases the exposable catalytic active sites.
The above process is further illustrated below with reference to specific examples.
Example 1:
1. dissolving 0.05g of carboxymethyl cellulose in 10ml of deionized water, then adding 0.26g of ammonium tetrathiomolybdate, stirring until the carboxymethyl cellulose is dissolved, then adding 0.5ml of isopropyl titanate, and stirring vigorously at room temperature for 24 hours to form a viscous mixture;
2. transferring the sticky mixture into a plastic mold, freezing for 5min by liquid nitrogen, and drying to obtain light gel;
3. placing the light gel in a high-temperature atmosphere furnace, heating to 150 ℃ at a speed of 5 ℃/min under the protection of nitrogen, preserving heat for 2h, heating to 900 ℃ at a speed of 2 ℃/min, preserving heat for 2h, and naturally cooling to room temperature to obtain the C-doped MoS 2 @TiO 2 An aerogel catalyst.
In this step, it should be noted that the light gel obtained by freeze drying is in the form of a lamellar structure aerogel under both macroscopic and microscopic conditions, the light gel is firstly calcined at a low temperature of 150 ℃ so as to be able to more completely retain the overall structure of the aerogel, and then slowly heated to 900 ℃ at a slow rate to carbonize the precursor. Aerogel structures are susceptible to collapse if the temperature is raised directly and rapidly to 900 ℃.
Example 2:
1. dissolving 0.2g of alginate in 10ml of deionized water, then adding 0.26g of ammonium tetrathiomolybdate, stirring until the ammonium tetrathiomolybdate is dissolved, then adding 1ml of tetrabutyl titanate, and violently stirring for 24 hours at room temperature to form a viscous mixture;
2. transferring the sticky mixture into a plastic mold, freezing for 10min by liquid nitrogen, and drying to obtain light gel;
3. putting the light gel in a high-temperature atmosphere furnace, and keeping the temperature in nitrogenUnder protection, firstly heating to 150 ℃ at the speed of 5 ℃/min, preserving heat for 2h, then heating to 900 ℃ at the speed of 2 ℃/min, preserving heat for 2h, and naturally cooling to room temperature to obtain C-doped MoS 2 @TiO 2 An aerogel catalyst.
Example 3:
1. dissolving 0.05g of polyacrylic acid in 10ml of deionized water, then adding a mixture of 0.26g of ammonium molybdate and thiourea, stirring until the mixture is dissolved, then adding 1ml of titanium tetrachloride, and vigorously stirring at room temperature for 24 hours to form a viscous mixture;
2. transferring the sticky mixture into a plastic mold, freezing for 20min by liquid nitrogen, and drying to obtain light gel;
3. placing the light gel in a high-temperature atmosphere furnace, heating to 150 ℃ at the speed of 5 ℃/min under the protection of nitrogen, preserving heat for 2h, heating to 900 ℃ at the speed of 2 ℃/min, preserving heat for 2h, and naturally cooling to room temperature to obtain C-doped MoS 2 @TiO 2 An aerogel catalyst.
Example 4:
1. dissolving 0.2g of polyethyleneimine in 10ml of deionized water, then adding a mixture of 0.26g of sodium molybdate and thioacetamide, stirring until the mixture is dissolved, then adding 1ml of titanium sulfate, and vigorously stirring at room temperature for 24 hours to form a viscous mixture;
2. transferring the sticky mixture into a plastic mold, freezing for 30min by liquid nitrogen, and drying to obtain light gel;
3. placing the light gel in a high-temperature atmosphere furnace, heating to 150 ℃ at the speed of 5 ℃/min under the protection of nitrogen, preserving heat for 2h, heating to 900 ℃ at the speed of 2 ℃/min, preserving heat for 2h, and naturally cooling to room temperature to obtain C-doped MoS 2 @TiO 2 An aerogel catalyst.
In the above examples, the mass of the biomass natural polysaccharide or the small molecule polymer is limited to the range of 0.05-0.2g, and it should be noted that if it is greater than 0.2g or less than 0.05g, the finally prepared catalyst is fragile, easy to collapse, and unable to form a gel structure, thereby increasing the difficulty of recovery.
FIG. 2 shows C-doped MoS 2 @TiO 2 XRD characterization pattern of aerogel catalyst, and its preparation methodComparing with the standard PDF card, it can be seen that, in FIG. 2, the diffraction peak is related to MoS 2 And TiO 2 The crystal structures correspond one to one, and TiO is found 2 The successful preparation of the catalyst was demonstrated for the standard rutile form.
C-doped MoS prepared from examples 1-4 above 2 @TiO 2 The aerogel catalyst, from the macroscopic morphology as shown in fig. 3, exhibits the morphological characteristics of an aerogel, being light and non-brittle. From the microscopic morphology as shown in fig. 4, it shows a stable layered structure connected with each other, and has a large specific surface area, increasing the exposable catalytic active sites, thus being able to overcome the problems of easy accumulation, easy blowing off and difficult recovery of the existing powder catalyst in the process of gas degradation of VOCs.
While the present disclosure has been described in detail with reference to specific embodiments, the above description of the embodiments is only for the purpose of facilitating understanding of the method and the core idea of the present disclosure, and those skilled in the art may change the embodiments and the application scope according to the idea of the present disclosure. Accordingly, the description should not be construed as limiting the disclosure.
Claims (8)
1. Preparation of C-doped MoS 2 @TiO 2 A method of making an aerogel catalyst, comprising the steps of:
s100: dissolving natural polysaccharide or micromolecular polymer of biomass in deionized water, and adding MoS 2 Precursor and TiO 2 Stirring the precursor at room temperature to obtain a viscous mixture;
s200: freezing and drying the viscous mixture to obtain light gel;
s300: calcining the light gel to obtain C-doped MoS 2 @TiO 2 An aerogel catalyst.
2. The method of claim 1, wherein the biomass natural polysaccharide or small molecule polymer has a mass of 0.05-0.2g in step S100.
3. The method of claim 1 or 2, wherein the biomass-natural polysaccharide comprises carboxymethyl cellulose and alginate.
4. The method of claim 1 or 2, wherein the small molecule polymer comprises polyacrylic acid and polyethyleneimine.
5. The method of claim 1, wherein the molybdenum sulfide precursor comprises any one of: ammonium tetrathiomolybdate, a mixture of ammonium molybdate and thiourea, and a mixture of sodium molybdate and thioacetamide.
6. The method of claim 1, wherein the TiO 2 The precursor comprises any one of the following components: tetrabutyl titanate, isopropyl titanate, titanium tetrachloride and titanium sulfate.
7. The method of claim 1, wherein the freezing time of the viscous mixture in step S200 is 5-30min.
8. The method as claimed in claim 1, wherein the calcination temperature of the light gel in the step S300 is 150-900 ℃.
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