CN105833859A - Preparation method for Bi serial amorphous catalyst loaded on carbon nano tube - Google Patents

Preparation method for Bi serial amorphous catalyst loaded on carbon nano tube Download PDF

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Publication number
CN105833859A
CN105833859A CN201610256890.1A CN201610256890A CN105833859A CN 105833859 A CN105833859 A CN 105833859A CN 201610256890 A CN201610256890 A CN 201610256890A CN 105833859 A CN105833859 A CN 105833859A
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carbon nano
solvent
mixed liquor
preparation
functionalization
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周丽娜
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Shanghai Dianji University
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Shanghai Dianji University
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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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/18—Arsenic, antimony or bismuth
    • 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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/18—Carbon
    • B01J21/185—Carbon nanotubes
    • 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
    • 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
    • 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
    • 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
    • B01J27/057—Selenium or tellurium; Compounds thereof
    • B01J27/0573—Selenium; Compounds thereof
    • 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
    • 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
    • B01J27/057—Selenium or tellurium; Compounds thereof
    • B01J27/0576—Tellurium; Compounds thereof

Abstract

The invention provides a preparation method for a Bi serial amorphous catalyst loaded on a carbon nano tube. The preparation method comprises the following steps: 1) dissolving a Bi-containing compound in a solvent; 2) dissolving the compound containing S, Se or Te in the solvent; 3) mixing a mixed liquor acquired in the step 1) with the mixed liquor acquired in the step 2) according to the stoichiometric ratio of the reactants; 4) adding a multi-wall carbon nano tube after functionalization and an alkaline conditioning agent into a mixture solution of the defined amount of deionized water and solvent, and ultrasonically dispersing to form black carbon pulp; 5) mixing the mixture solutions acquired in the step 3) and step 4) at a certain ratio and transferring to a microwave reactor for reacting; and 6) after ending the reaction, processing, collecting the solid products and drying, thereby acquiring the Bi serial amorphous catalyst loaded on the carbon nano tube. According to the preparation method provided by the invention, the catalytic performance of the carbon material can be promoted, and the application scope of the Bi-containing compound in the fields of catalysis, energy storage, phase change storage, thermoelectricity, and the like can be widened.

Description

A kind of preparation method of carbon nanotube loaded Bi series amorphous catalyst
Technical field
The present invention relates to the preparation method of a kind of carbon nanotube loaded amorphous catalyst.
Background technology
Atom in amorphous alloy compound has the arrangement architecture of shortrange order, longrange disorder, its surface Atom as catalytic reaction activity center is evenly distributed, and character is identical；And it is permissible by its composition of modulation Efficiently control its electronic property, obtain suitable catalytic active center.Amorphous alloy catalyst above-mentioned Good characteristic be conventional crystal alloy catalyst incomparable, thus once come out just be applied to catalysis Many aspects of process.
The amorphous compound that Bi Yu VIA major element is formed, such as Bi2O3、Bi2S3、Bi2Se3And Bi2Te3 Etc. can be used as visible light catalyst, and energy storage material, thermoelectric material, phase transformation store material and topology insulation Body etc..It addition, CNT owing to nanoscale, specific surface area are big, the key state on surface and electronic state with Intragranular portion is different, surface atom is coordinated the congruent active position causing surface increases, and this just makes it possess Primary condition as catalyst.Meanwhile, CNT has the tube wall of graphite-like structure of uniqueness and special Vestibule space so that it shows extremely excellent adsorption and desorption performance to reactant and product.And Compared with conventional catalyst carrier, carbon nano tube compound material mechanical strength is high, electric property is good.Carbon is received The Bi series amorphous state composite catalyst of mitron load, can effectively combine CNT and Bi series amorphous The advantage of state catalyst, it would be possible to the developing for many catalytic applications brings new opportunity.At present, There is no this type of report.
Summary of the invention
The present invention provides a kind of simplicity, quickly prepares carbon nanotube loaded Bi series amorphous catalyst Method, with the drawbacks described above overcoming prior art to exist.
The preparation method of the Bi series amorphous catalyst that the present invention is carbon nanotube loaded, comprises the steps:
1) by the compound dissolution containing Bi element in solvent, heating, mechanical agitation；
2) by the compound dissolution containing S, Se or Te element in solvent, heating, ultrasonic disperse；
3) according to Bi2S3、Bi2Se3Or Bi2Te3Bi:S's or Bi:Se determined by chemical composition or Bi:Te Mol ratio is 2:3, by step 1) mixed liquor and step 2) mixed liquor mix, mechanical agitation；
4) multi-walled carbon nano-tubes after functionalization and alkaline conditioner are added the mixed of appropriate amount of deionized water and solvent Close in solution, ultrasonic disperse, until CNT is uniformly dispersed, form black carbon slurry；
5) by the multi-walled carbon nano-tubes after described functionalization and Bi2S3、Bi2Se3Or Bi2Te3Mass ratio be 0.2:1-3:1, by step 3) with step 4) mixed liquor mix, mechanical agitation, be transferred to microwave reactor In, it is heated to 135-150 DEG C under mechanical stirring and reacts 0.5-2 hour；
6) collect solid product through post-processing step after reaction terminates, obtain described carbon nanotube loaded after drying Bi series amorphous catalyst.Described post-processing step includes removing reactant liquor sample centrifugation, washing Remove solvent and other by-products.
The described compound containing Bi element be the chloride containing Bi element, oxide, sulfate, nitrate or Carbonate, the preferably nitrate containing Bi element.
The described compound containing S element, selected from thioacetamide, sodium thiosulfate, thiourea or sodium sulfide etc., Preferably thioacetamide；The described compound containing Se or Te element be the chloride containing Se or Te element, Oxide, sulfate, nitrate, nitrite or carbonate, the preferably oxide containing Se or Te element.
Multi-walled carbon nano-tubes after described functionalization, refers to through oxidizing, after purification, then through network The multi-walled carbon nano-tubes that mixture functionalization processes.Processing method can be found in: Jiao Zhihui, Zhang Xiaobin, Cheng Jipeng, " preparation of CNT/ZnS composite and performance characterization thereof ", Journal of Inorganic Materials, Vol.23, No.3 (2008), the 491-495 page.
Preferably, the multi-walled carbon nano-tubes after described functionalization uses ultrasonic mode to disperse in a solvent, institute State solvent and can select the Conventional solvents of this area, such as, 1,2-PD, 1,3-PD, butanediol, Glycerol and ethylene glycol, preferably ethylene glycol.
Described alkaline conditioner, refer to various make solution present pH value more than 7 material, including all kinds of nothings Machine alkali and organic base and various alkaline matter, such as sodium hydroxide, potassium hydroxide, ammonia, sodium carbonate, carbon Acid hydrogen sodium etc..Step 4) addition of neutral and alkali regulator is so that the pH value of mixed liquor is 10-14.
The preparation method of the carbon nanotube loaded Bi series amorphous catalyst of the present invention, both can improve carbon The catalytic performance of material, can widen again containing Bi compound in fields such as catalysis, energy storage, phase transformation storage, thermoelectricity Range of application.The chemical plating method used during preparation, imparts the specific surface that catalyst is bigger, improves The degree of scatter of active component, thus improve the heat stability of catalyst, make amorphous alloy catalyst Industrial prospect is brighter and clearer.Chemical plating synthesis technique simple flow, reaction is quickly, it is easy to control, and adapts to Extensive commercial production.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of embodiment 1 product.
Fig. 2 is the EDS collection of illustrative plates of embodiment 4 product.
Fig. 3 is the TEM image of embodiment 4 product.
Detailed description of the invention
Provide present pre-ferred embodiments below in conjunction with the accompanying drawings, to describe technical scheme in detail.
Embodiment 1
1) a certain amount of Bi (NO is weighed3)3·5H2O, is dissolved in ethylene glycol, and heats, and makes 0.5mol/l Solution, mechanical agitation.
2) weigh the NaOH of the multi-walled carbon nano-tubes after 0.16g functionalization and 5g, measure 17mL's respectively Deionized water and the ethylene glycol of 53mL, be dissolved in pressed powder in the mixed solution of deionized water and ethylene glycol, Ultrasonic disperse, until CNT is uniformly dispersed, forms black carbon slurry.
3) take step 1) in solution 4mL, with step 2) mixed liquor mix, mechanical agitation.Transfer To the three-neck flask of microwave reactor, being heated to 145 DEG C, mechanical agitation, speed is 800r/min, instead Answer 30min.
4) after reaction terminates, centrifugation, wash, collect solid product, dry.
Using the thing phase of X-ray polycrystalline diffractometer assay products, result is the carbon nanotube loaded of widthization Bi2O3The diffraction maximum of amorphous catalyst.(see Fig. 1)
Embodiment 2
1) a certain amount of Bi (NO is weighed3)3·5H2O, is dissolved in ethylene glycol, and heats, and makes 0.6mol/l Solution, mechanical agitation.
2) weigh a certain amount of thioacetamide, be dissolved in ethylene glycol, and heat, make the molten of 0.8mol/l Liquid, mechanical agitation.
3) according to Bi2S3Mol ratio 2:3 of Bi:S determined by chemical composition, by step 1) and step 2) Solution mixing, mechanical agitation.
4) weigh the KOH of the multi-walled carbon nano-tubes after 0.20g functionalization and 5g, measure 20mL's respectively Deionized water and the ethylene glycol of 50mL, be dissolved in pressed powder in the mixed solution of deionized water and ethylene glycol, Ultrasonic disperse, until CNT is uniformly dispersed, forms black carbon slurry.
5) take step 3) in solution 5mL, with step 2) mixed liquor mix, mechanical agitation.Transfer To the three-neck flask of microwave reactor, being heated to 135 DEG C, mechanical agitation, speed is 800r/min, instead Answer 30min.
6) after reaction terminates, centrifugation, wash, collect solid product, dry.
Using the thing phase of X-ray polycrystalline diffractometer assay products, result is the carbon nanotube loaded of widthization Bi2S3The diffraction maximum of amorphous catalyst.
Embodiment 3
1) a certain amount of Bi (NO is weighed3)3·5H2O, is dissolved in ethylene glycol, and heats, and makes 0.2mol/l Solution, mechanical agitation.
2) a certain amount of Na is weighed2SeO3, it is dissolved in ethylene glycol, and heats, make the solution of 0.2mol/l, Mechanical agitation.
3) according to Bi2Se3Mol ratio 2:3 of Bi:Se determined by chemical composition, by step 1) and step 2) Solution mixing, mechanical agitation.
4) weigh the NaOH of the multi-walled carbon nano-tubes after 0.20g functionalization and 5g, measure 20mL's respectively Deionized water and the ethylene glycol of 50mL, be dissolved in pressed powder in the mixed solution of deionized water and ethylene glycol, Ultrasonic disperse, until CNT is uniformly dispersed, forms black carbon slurry.
5) take step 3) in solution 6mL, with step 2) mixed liquor mix, mechanical agitation.Transfer To the three-neck flask of microwave reactor, being heated to 150 DEG C, mechanical agitation, speed is 800r/min, instead Answer 30min.
6) after reaction terminates, centrifugation, wash, collect solid product, dry.
Using the thing phase of X-ray polycrystalline diffractometer assay products, result is the carbon nanotube loaded of widthization Bi2Se3The diffraction maximum of amorphous catalyst.
Embodiment 4
1) a certain amount of Bi (NO is weighed3)3·5H2O, is dissolved in ethylene glycol, and heats, and makes 0.5mol/l Solution, mechanical agitation.
2) a certain amount of Na is weighed2TeO3, it is dissolved in ethylene glycol, and heats, make the solution of 0.5mol/l, Mechanical agitation.
3) according to Bi2Te3Mol ratio 2:3 of Bi:Te determined by chemical composition, by step 1) and step 2) Solution mixing, mechanical agitation.
4) weigh the NaOH of the multi-walled carbon nano-tubes after 0.18g functionalization and 5g, measure 20mL's respectively Deionized water and the ethylene glycol of 50mL, be dissolved in pressed powder in the mixed solution of deionized water and ethylene glycol, Ultrasonic disperse, until CNT is uniformly dispersed, forms black carbon slurry.
5) take step 3) in solution 5mL, with step 2) mixed liquor mix, mechanical agitation.Transfer To the three-neck flask of microwave reactor, being heated to 150 DEG C, mechanical agitation, speed is 800r/min, instead Answer 30min.
6) after reaction terminates, centrifugation, wash, collect solid product, dry.
Using the thing phase of X-ray polycrystalline diffractometer assay products, result is the carbon nanotube loaded of widthization Bi2Te3The diffraction maximum of amorphous catalyst.Use energy disperse spectroscopy that product carries out elementary analysis, find except containing C, Cu (both of which, from the copper mesh of band carbon film, is the support film of sample) outward, mainly contain Bi and Te unit Element (see Fig. 2).Use the micro structure of transmission electron microscopy observation product, find that the surface of CNT is attached One layer of densification and the most noncrystal (see Fig. 3).

Claims (9)

1. the preparation method of a carbon nanotube loaded Bi series amorphous catalyst, it is characterised in that Comprise the steps:
1) by the compound dissolution containing Bi element in solvent；
2) by the compound dissolution containing S, Se or Te element in solvent；
3) according to Bi2S3、Bi2Se3Or Bi2Te3Bi:S's or Bi:Se determined by chemical composition or Bi:Te Mol ratio is 2:3, by step 1) mixed liquor and step 2) mixed liquor mix；
4) multi-walled carbon nano-tubes after functionalization and alkaline conditioner are added the mixed of appropriate amount of deionized water and solvent Close in solution, ultrasonic disperse, form black carbon slurry；
5) by the multi-walled carbon nano-tubes after described functionalization and Bi2S3、Bi2Se3Or Bi2Te3Mass ratio be 0.2:1-3:1, by step 3) with step 4) mixed liquor mix, mechanical agitation, be transferred to microwave reactor In, it is heated to 135-150 DEG C under mechanical stirring and reacts 0.5-2 hour；
6) collect solid product through post-processing step after reaction terminates, obtain described carbon nanotube loaded after drying Bi series amorphous catalyst.
2. the method for claim 1, it is characterised in that the multi-walled carbon nano-tubes after described functionalization It is through oxidizing, after purification, then the CNT processed through chelating agent functionalization.
3. the method for claim 1, it is characterised in that the described compound containing Bi element is to contain The chloride of Bi element, oxide, sulfate, nitrate or carbonate, the preferably nitrate containing Bi element.
4. the method for claim 1, it is characterised in that the described compound containing Bi element is to contain The nitrate of Bi element.
5. the method for claim 1, it is characterised in that the described compound containing S element, is selected from Thioacetamide, sodium thiosulfate, thiourea or sodium sulfide；The described compound containing Se or Te element is to contain The chloride of Se or Te element, oxide, sulfate, nitrate, nitrite or carbonate.
6. the method for claim 1, it is characterised in that the described compound containing S element is sulfur generation Acetamide；The described compound containing Se or Te element is the oxide containing Se or Te element.
7. the method for claim 1, it is characterised in that described solvent is ethylene glycol.
8. the method for claim 1, it is characterised in that described alkaline conditioner refers to various making Solution presents the pH value material more than 7.
9. method as claimed in claim 8, it is characterised in that described alkaline conditioner selected from sodium hydroxide, Potassium hydroxide, ammonia, sodium carbonate or sodium bicarbonate, the addition of described alkaline conditioner is for making mixed liquor PH value be 10-14.
CN201610256890.1A 2016-04-22 2016-04-22 Preparation method for Bi serial amorphous catalyst loaded on carbon nano tube Pending CN105833859A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106252661A (en) * 2016-10-14 2016-12-21 成都理工大学 Bismuth sulfide/carbon nano tube compound material and its preparation method and application
CN113398904A (en) * 2021-05-06 2021-09-17 桂林电子科技大学 Preparation method and application of catalyst for medium-low temperature photo-thermoelectric synergistic catalytic oxidation of VOCs (volatile organic compounds)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106252661A (en) * 2016-10-14 2016-12-21 成都理工大学 Bismuth sulfide/carbon nano tube compound material and its preparation method and application
CN113398904A (en) * 2021-05-06 2021-09-17 桂林电子科技大学 Preparation method and application of catalyst for medium-low temperature photo-thermoelectric synergistic catalytic oxidation of VOCs (volatile organic compounds)

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Application publication date: 20160810