WO2023272413A1 - Application d'un nanocatalyseur à base de disulfure d'étain dans la production d'hydrogène par décomposition catalytique piézoélectrique de l'eau - Google Patents

Application d'un nanocatalyseur à base de disulfure d'étain dans la production d'hydrogène par décomposition catalytique piézoélectrique de l'eau Download PDF

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Publication number
WO2023272413A1
WO2023272413A1 PCT/CN2021/102591 CN2021102591W WO2023272413A1 WO 2023272413 A1 WO2023272413 A1 WO 2023272413A1 CN 2021102591 W CN2021102591 W CN 2021102591W WO 2023272413 A1 WO2023272413 A1 WO 2023272413A1
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Prior art keywords
tin
tin disulfide
nanoflowers
water
catalyst
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PCT/CN2021/102591
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English (en)
Chinese (zh)
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路建美
李娜君
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苏州大学
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Priority to PCT/CN2021/102591 priority Critical patent/WO2023272413A1/fr
Publication of WO2023272413A1 publication Critical patent/WO2023272413A1/fr

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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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Definitions

  • the invention relates to the technical field of inorganic nanomaterials and piezoelectric catalysis, in particular to a preparation method of copper ion/silver ion doped tin disulfide nanoflowers and its application in piezoelectric catalytic decomposition of water to produce hydrogen.
  • Hydrogen is an efficient and clean green energy. As a fuel, it has the advantages of rich raw materials, high combustion value, and clean and pollution-free combustion products.
  • the existing technology uses solar energy to realize the photocatalytic water decomposition of semiconductors to produce hydrogen.
  • perovskite oxide With unique physical and chemical properties, it is widely used in water splitting to produce hydrogen to realize the development of new energy and the purification of the environment. It is a green and environmentally friendly photocatalytic material with good development prospects.
  • the conditions required for photocatalysis are more complicated and the energy consumption is larger.
  • the prior art discloses the application of tin disulfide/carbon nanofiber composite materials in the degradation of organic pollutants.
  • Precursor solution dry after reaction to obtain tin disulfide/carbon nanofiber composite material, put tin disulfide/carbon nanofiber composite material into water containing organic pollutants, and then ultrasonically treat organic pollutants in water remove.
  • the application effect of the catalyst in hydrogen production from water splitting is not disclosed.
  • the invention provides an inorganic nanometer material of copper ion/silver ion doped tin disulfide nanoflowers and a preparation method thereof, which realizes the purpose of catalytically decomposing water to produce hydrogen through ultrasonic treatment under the condition of not needing light.
  • the present invention adopts the following specific technical scheme: the application of tin disulfide nano-catalyst in decomposing water to produce hydrogen.
  • the method for decomposing water with a tin disulfide nano catalyst to produce hydrogen comprises the following steps: placing the tin disulfide nano catalyst in water added with a sacrificial agent, and then performing ultrasonic treatment to realize decomposing water to produce hydrogen, and detecting the generation of hydrogen through gas chromatography.
  • the sacrificial agent is sodium sulfite.
  • the tin disulfide nano catalyst is copper ion doped tin disulfide nanoflower or silver ion doped tin disulfide nanoflower.
  • the precursor solution containing tin source and sulfur source is subjected to solvothermal reaction, centrifuged, washed, and dried to obtain tin disulfide nanoflowers.
  • a copper source is placed in a precursor solution containing a tin source and a sulfur source, centrifuged and washed after solvothermal reaction, and dried to obtain copper ion-doped tin disulfide nanoflowers.
  • a silver source is placed in a precursor solution containing a tin source and a sulfur source, centrifuged and washed after solvothermal reaction, and dried to obtain silver ion-doped tin disulfide nanoflowers.
  • pure tin disulfide nanoflowers SnS 2
  • copper ion doped tin disulfide nanoflowers Cu-SnS 2
  • silver ion doped tin disulfide nanoflowers Ag-SnS 2
  • the copper ion or silver ion doped tin disulfide nanoflowers provided by the present invention improve the utilization rate of free carriers, and can also promote the separation of free carriers to realize the catalytic reaction under the condition of no light.
  • tin tetrachloride pentahydrate (SnCl 4 5H 2 O) is used as the tin source
  • thioacetamide (CH 3 CSNH 2 ) is used as the sulfur source
  • the molar ratio of SnCl 4 ⁇ 5H 2 O to CH 3 CSNH 2 is 1: (1-10), such as 1:1-1:8, preferably, SnCl 4 ⁇ 5H 2 O and CH 3 CSNH 2
  • the molar ratio is 1:4.
  • the solvothermal reaction is carried out in a reactor at 100-160° C. for 6-24 hours, preferably at 120° C. for 12 hours.
  • a copper source is added as a dopant to prepare copper ion-doped tin disulfide nanoflowers (Cu-SnS 2 ).
  • copper nitrate trihydrate Cu(NO 3 ) 2 ⁇ 3H 2 O
  • the molar fraction of copper ions relative to tin ions is 1%-15%, preferably 3%-6%.
  • a silver source is added as a dopant to prepare silver ion-doped tin disulfide nanoflowers (Ag-SnS 2 ).
  • silver nitrate (AgNO 3 ) is selected as the silver source, and the mole fraction of silver ions relative to tin ions is 1%-15%, preferably 3%-6%.
  • sodium sulfite Na 2 SO 3
  • the frequency of ultrasonic treatment is 40-60KHz
  • the power is 400-800W, preferably 45KHz, 600W. Further, during the ultrasonic treatment, no light is used, and it is carried out under the condition of completely avoiding light.
  • the present invention discloses a preparation method of an inorganic nanometer material that decomposes water and produces hydrogen by using mechanical energy vibration without illumination.
  • the central symmetry of the crystal structure is a key factor affecting piezoelectricity, and ion doping is currently a feasible way to improve piezoelectricity.
  • the present invention utilizes the difference in ionic radius and the formation of an amorphous layer, and incorporates copper ions or silver ions into tin disulfide nanoflowers through a simple solvothermal method to improve the piezoelectricity of SnS 2 , and the two synergistically improve piezoelectric catalytic performance.
  • Figure 1 is a scanning electron microscope image of pure SnS 2 nanoflowers.
  • Figure 2 is a scanning electron microscope image of 3% Cu-SnS 2 nanoflowers.
  • Figure 3 is a scanning electron microscope image of 3%Ag-SnS 2 nanoflowers.
  • Figure 4 is the PFM piezoelectric response butterfly curve of SnS 2 .
  • Fig. 5 is Cu-SnS 2 PFM piezoelectric response butterfly curve.
  • Fig. 6 is the piezoelectric response butterfly curve of Ag-SnS 2 PFM.
  • Fig. 7 is an effect diagram of SnS 2 , Cu-SnS 2 , Ag-SnS 2 piezoelectric catalytic decomposition of water to produce hydrogen.
  • the present invention obtains simple SnS 2 nanoflowers, copper ion or silver ion doped SnS 2 nanoflowers (Cu-SnS 2 , Ag-SnS 2 ) through a simple solvothermal method, and realizes decomposing aquatic products without light. purpose of hydrogen.
  • the copper ion or silver ion doped tin disulfide nanoflower inorganic nanomaterial provided by the invention improves the utilization rate of free carriers, and realizes catalytic reaction efficiently under the condition of no light.
  • the mole fraction of copper ions or silver ions relative to tin ions is taken as a percentile.
  • Example 1 The preparation of pure SnS 2 nanoflowers, the specific steps are as follows: the molar ratio of SnCl 4 5H 2 O to CH 3 CSNH 2 is 1:4, and 0.5 mmol (175.3 mg) SnCl 4 5H 2 O and 2 Mmol (150.0 mg) CH 3 CSNH 2 were dissolved in 20 mL of absolute ethanol respectively, the two solutions were mixed evenly and placed in a 50 mL reactor liner, and reacted at 120°C for 12 hours. After the reaction, the obtained product was washed with deionized water and ethanol three times in sequence, and finally dried at 60°C for 12 hours to obtain SnS 2 nanoflowers.
  • Accompanying drawing 1 is the scanning electron microscope picture of above-mentioned simple SnS 2 nanoflower. It can be seen from the figure that pure SnS 2 is interspersed with large nanosheets to form a nanoflower morphology.
  • Example 2 Preparation of 3% Cu-SnS 2 nanoflowers, the specific steps are as follows: the molar fraction of copper ions is 3% of Sn 4+ , and 0.015 mmol (3.62 mg) Cu(NO 3 ) 2 ⁇ 3H 2 O is dissolved In 5 mL absolute ethanol, 0.48 mmol (170.0 mg) SnCl 4 ⁇ 5H 2 O was dissolved in 15 mL absolute ethanol, 150 mg (2 mmol) CH 3 CSNH 2 was dissolved in 20 mL absolute ethanol, and the above three The two solutions were mixed evenly and placed in a 50 mL reactor liner, and reacted at 120 °C for 12 hours.
  • Example 3 Preparation of 6% Cu-SnS 2 nanoflowers, the specific steps are as follows: the molar fraction of copper ions is 6% of Sn 4+ , and 0.03 mmol (7.25 mg) Cu(NO 3 ) 2 ⁇ 3H 2 O is dissolved In 5 mL absolute ethanol, 0.47 mmol (164.8 mg) SnCl 4 ⁇ 5H 2 O was dissolved in 15 mL absolute ethanol, 150 mg (2 mmol) CH 3 CSNH 2 was dissolved in 20 mL absolute ethanol, and the above After the three solutions were mixed evenly, they were placed in a 50 mL reactor liner and reacted at 120 °C for 12 hours. After the reaction, the obtained product was washed with deionized water and ethanol three times in sequence, and finally dried at 60° C. for 12 hours to obtain Cu-SnS 2 nanoflowers.
  • Example 4 Preparation of 9% Cu-SnS 2 nanoflowers, the specific steps are as follows: the molar fraction of copper ions is 9% of Sn 4+ , and 0.045 mmol (10.87 mg) Cu(NO 3 ) 2 ⁇ 3H 2 O is dissolved In 5 mL absolute ethanol, 0.455 mmol (159.5 mg) SnCl 4 ⁇ 5H 2 O was dissolved in 15 mL absolute ethanol, 150 mg (2 mmol) CH 3 CSNH 2 was dissolved in 20 mL absolute ethanol, the above three The two solutions were mixed evenly and placed in a 50 mL reactor liner, and reacted at 120 °C for 12 hours. After the reaction, the obtained product was washed with deionized water and ethanol three times in sequence, and finally dried at 60° C. for 12 hours to obtain Cu-SnS 2 nanoflowers.
  • Example 5 The preparation of 1% Ag-SnS 2 nanoflowers, the specific steps are as follows: the molar fraction of silver ions is 1% of Sn 4+ , 0.005 mmol (0.85 mg) AgNO 3 is dissolved in 5 mL of absolute ethanol, 0.495 mmol (173.6 mg) SnCl 4 5H 2 O was dissolved in 15 mL of absolute ethanol, 150 mg (2 mmol) of CH 3 CSNH 2 was dissolved in 20 mL of absolute ethanol, the above three solutions were mixed uniformly and placed in In a 50 mL reactor liner, react at 120°C for 12 hours. After the reaction, the product obtained was washed with deionized water and ethanol three times in sequence, and finally dried at 60° C. for 12 hours to obtain Ag-SnS 2 nanoflowers.
  • Example 6 The preparation of 3% Ag-SnS 2 nanoflowers, the specific steps are as follows: the molar fraction of silver ions is 3% of Sn 4+ , 0.015 mmol (2.55 mg) AgNO 3 is dissolved in 5 mL of absolute ethanol, 0.48 mmol (170.0 mg) SnCl 4 5H 2 O was dissolved in 15 mL of absolute ethanol, 150 mg (2 mmol) of CH 3 CSNH 2 was dissolved in 20 mL of absolute ethanol, the above three solutions were mixed uniformly and placed in In a 50 mL reactor liner, react at 120°C for 12 hours.
  • Example 7 The preparation of 6% Ag-SnS 2 nanoflowers, the specific steps are as follows: the molar fraction of silver ions is 6% of Sn 4+ , 0.03 mmol (5.10 mg) AgNO 3 is dissolved in 5 mL of absolute ethanol, 0.47 mmol (164.8 mg) SnCl 4 5H 2 O was dissolved in 15 mL of absolute ethanol, 150 mg (2 mmol) of CH 3 CSNH 2 was dissolved in 20 mL of absolute ethanol, the above three solutions were mixed uniformly and placed in In a 50 mL reactor liner, react at 120°C for 12 hours. After the reaction, the product obtained was washed with deionized water and ethanol three times in sequence, and finally dried at 60° C. for 12 hours to obtain Ag-SnS 2 nanoflowers.
  • Example 8 The preparation of 9% Ag-SnS 2 nanoflowers, the specific steps are as follows: the molar fraction of silver ions is 9% of Sn 4+ , 0.045 mmol (7.64 mg) AgNO 3 is dissolved in 5 mL of absolute ethanol, 0.455 mmol (159.5) SnCl 4 5H 2 O was dissolved in 15 mL of absolute ethanol, 150 mg (2 mmol) of CH 3 CSNH 2 was dissolved in 20 mL of absolute ethanol, the above three solutions were mixed uniformly and placed in 50 In the liner of a mL reactor, react at 120°C for 12 hours. After the reaction, the product obtained was washed with deionized water and ethanol three times in sequence, and finally dried at 60° C. for 12 hours to obtain Ag-SnS 2 nanoflowers.
  • Embodiment 9 In order to study the difference among the three, the piezoelectricity of the three samples is characterized by PFM testing.
  • the results of accompanying drawings 4 to 6 show that the three samples have obtained typical Butterfly rings, these results confirm the piezoelectric properties of the three samples synthesized. From Figures 4 to 6, it can be seen that the maximum amplitudes of SnS 2 , 3%Cu-SnS 2 and 3%Ag-SnS 2 are 15 pm, 30 pm and 45 pm respectively. Obviously, Ag-SnS 2 exhibits the highest Piezoelectric response magnitude.
  • Example 10 SnS 2 piezoelectric catalytic decomposition of water to produce hydrogen: 10 mg of SnS 2 nanoflowers were dispersed in 10 mL of Na 2 SO 3 aqueous solution (0.05 M), and Na 2 SO 3 was used as a sacrificial agent. Seal the above suspension in a 30 mL borosilicate tube to evacuate and purge with Ar for about 5 min to completely remove the air. Then place the borosilicate tube in the center of the ultrasonic cleaner, and turn on the ultrasound (45 KHz, 600 W) in the dark to decompose water and produce hydrogen.
  • 10 mg of SnS 2 nanoflowers were dispersed in 10 mL of Na 2 SO 3 aqueous solution (0.05 M), and Na 2 SO 3 was used as a sacrificial agent. Seal the above suspension in a 30 mL borosilicate tube to evacuate and purge with Ar for about 5 min to completely remove the air. Then place the borosilicate tube in the center of the ultra
  • Example 11 Cu-SnS 2 piezoelectric catalytic decomposition of water to produce hydrogen: 10 mg 3% Cu-SnS 2 nanoflowers were dispersed in 10 mL Na 2 SO 3 aqueous solution (0.05 M), and Na 2 SO 3 was used as a sacrificial agent. Seal the above suspension in a 30 mL borosilicate tube to evacuate and purge with Ar for about 5 min to completely remove the air. Then place the borosilicate tube in the center of the ultrasonic cleaner, and turn on the ultrasound (45 KHz, 600 W) in the dark to decompose water and produce hydrogen.
  • 10 mg 3% Cu-SnS 2 nanoflowers were dispersed in 10 mL Na 2 SO 3 aqueous solution (0.05 M), and Na 2 SO 3 was used as a sacrificial agent. Seal the above suspension in a 30 mL borosilicate tube to evacuate and purge with Ar for about 5 min to completely remove the air. Then place the borosilicate tube
  • Example 12 Ag-SnS 2 piezoelectric catalyzed water splitting hydrogen production experiment: 10 mg 3% Ag-SnS 2 nanoflowers were dispersed in 10 mL Na 2 SO 3 aqueous solution (0.05 M), and Na 2 SO 3 was used as a sacrificial agent. Seal the above suspension in a 30 mL borosilicate tube to evacuate and purge with Ar for about 5 min to completely remove the air. Then place the borosilicate tube in the center of the ultrasonic cleaner, and turn on the ultrasound (45 KHz, 600 W) in the dark to decompose water and produce hydrogen.
  • 10 mg 3% Ag-SnS 2 nanoflowers were dispersed in 10 mL Na 2 SO 3 aqueous solution (0.05 M), and Na 2 SO 3 was used as a sacrificial agent. Seal the above suspension in a 30 mL borosilicate tube to evacuate and purge with Ar for about 5 min to completely remove the air. Then place the borosilicate tube in
  • Comparative example 1 Take the 0.5-SnS 2 /CNFs (10 mg) composite material prepared in Example 3 of the prior art CN202010815126X to replace the 10 mg Ag-SnS 2 in Example 12, and keep the rest unchanged. As a comparative experiment, the results show that in The amount of H 2 generated in 4 hours was 275 ⁇ mol g -1 .
  • Comparative example 2 using photoreduction reaction to deposit silver nanoparticles on the surface of SnS 2 nanoflowers. Put 0.5 g of SnS into a beaker filled with 25 mL of AgNO solution (0.02 M ). Place the beaker under UV light with constant stirring. Then the powder was washed and separated by a centrifuge and dried at room temperature to prepare SnS 2 nanoflowers deposited by silver nanoparticles. Take 10 mg to replace the 10 mg Ag-SnS 2 in Example 12, and keep the rest unchanged as a comparative experiment , the results showed that the amount of H 2 generated within 4 hours was 285 ⁇ mol g -1 .
  • the catalytic performance is not significantly affected by replacing the metal dopant copper salt with copper acetate monohydrate (Cu(CO 2 CH 3 ) 2 ⁇ H 2 O).
  • the 3% Cu-SnS 2 prepared in Reference Example 2 produced 307 ⁇ mol g -1 of H 2 within 4 hours.
  • the piezoelectric effect builds a built-in electric field, realizes the effective separation of carriers, and improves the piezoelectric catalytic efficiency.
  • the present invention prepares tin disulfide nanoflowers (Cu-SnS 2 , Ag-SnS 2 ) doped with copper ions or silver ions by a simple solvothermal method and applies them to the field of piezoelectric catalysis for the first time.
  • the doping synergistically increases the sensitivity of the material to sense mechanical energy, improves the piezoelectricity, and thus enhances the catalytic performance.

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Abstract

L'invention concerne une application d'un nanocatalyseur à base de disulfure d'étain dans la production d'hydrogène par décomposition catalytique piézoélectrique de l'eau. Dans l'état de la technique, l'énergie solaire est utilisée pour obtenir une décomposition photocatalytique de l'eau d'un semiconducteur en vue de produire de l'hydrogène, mais les conditions exigées par la photocatalyse sont relativement complexes et la consommation d'énergie est relativement élevée. La présente invention concerne un nanomatériau inorganique d'une nanofleur de disulfure d'étain dopé aux ions cuivre ou aux ions argent. L'objet de décomposition catalytique de l'eau pour produire de l'hydrogène est obtenu au moyen d'un traitement par ultrasons sans nécessiter d'éclairage.
PCT/CN2021/102591 2021-06-27 2021-06-27 Application d'un nanocatalyseur à base de disulfure d'étain dans la production d'hydrogène par décomposition catalytique piézoélectrique de l'eau WO2023272413A1 (fr)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116099551A (zh) * 2023-02-07 2023-05-12 昆明理工大学 一种碳纳米管复合材料的制备方法及应用
CN116395751A (zh) * 2023-03-29 2023-07-07 哈尔滨理工大学 一种钐掺杂铁酸铋纳米材料的制备及压电催化应用
CN116395751B (zh) * 2023-03-29 2024-08-13 哈尔滨理工大学 一种钐掺杂铁酸铋纳米材料的制备及压电催化应用

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