CN114272939A - Hydrothermal synthesis Ni-doped CdS composite photocatalyst and preparation method and application thereof - Google Patents
Hydrothermal synthesis Ni-doped CdS composite photocatalyst and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a hydrothermal synthesis Ni-doped CdS composite photocatalyst, and a preparation method and application thereof, wherein the composite photocatalyst comprises the following components in proportion of (1-2) to (0.4-1): (10-20) CdS powder, nickel chloride hexahydrate and urea. The preparation method comprises the following steps of 1, weighing cadmium acetate and thioacetamide according to the proportion of (0.5-0.8) to (0.6-1.2), adding ethylenediamine and ethylene glycol according to the proportion of (1-4) to 1, and stirring to form a solution A; step 2, carrying out hydrothermal reaction on the solution A, and filtering to obtain CdS powder; step 3, mixing the components in the ratio of (1-2) to (0.4-1): (10-20) adding the CdS powder, nickel chloride hexahydrate and urea into deionized water, and stirring to obtain a solution B; and 4, carrying out hydrothermal reaction on the solution B, filtering and drying to obtain the Ni-doped CdS composite photocatalyst material.
Description
Technical Field
The invention belongs to the field of photocatalytic materials, and particularly belongs to a Ni-doped CdS composite photocatalyst synthesized by a hydrothermal method and a preparation method and application thereof.
Background
Energy shortage and environmental pollution are problems facing all countries around the world at present and needing to be solved urgently. The fossil energy accumulated in the earth for hundreds of millions of years is exploited and used in large scale in the last two hundred years, and the produced pollutants are released into the natural environment while the large amount of fossil energy is consumed. Nowadays, the photocatalytic technology is one of the effective ways to solve the environmental and energy problems.
CdS, a typical transition metal sulfide semiconductor, is one of the most interesting photocatalysts at present due to its appropriate band gap width (2.4ev) conduction band position and good visible light response. But the improvement of the photocatalytic efficiency is seriously hindered due to the rapid recombination of electron and hole pairs in the CdS and the self-serious photo-corrosion phenomenon.
At present, some researchers use light deposition to load noble metals such as gold, silver, platinum and the like on the surface of a semiconductor to improve the photocatalytic hydrogen production performance and stability of CdS. However, the noble metal is expensive and not suitable for large-area popularization, so other methods need to be found.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a composite photocatalyst of hydrothermally synthesized Ni-doped CdS, a preparation method and application thereof.
In order to achieve the purpose, the invention provides the following technical scheme:
the hydrothermally synthesized Ni-doped CdS composite photocatalyst comprises the following components in parts by weight (1-2) to (0.4-1): (10-20) CdS powder, nickel chloride hexahydrate and urea.
Preferably, the hydrothermally synthesized Ni-doped CdS composite photocatalyst is synthesized through a hydrothermal reaction.
A preparation method of a Ni-doped CdS composite photocatalyst by hydrothermal synthesis comprises the following processes,
step 3, mixing the components in the ratio of (1-2) to (0.4-1): (10-20) adding the CdS powder, nickel chloride hexahydrate and urea into deionized water, and stirring to obtain a solution B;
and 4, carrying out hydrothermal reaction on the solution B, filtering and drying to obtain the Ni-doped CdS composite photocatalyst material.
Preferably, in the step 1, the stirring process is to obtain the transparent solution A after stirring for 0.5 to 2 hours at a speed of 500 to 800r/min by a magnetic stirrer.
Preferably, in the step 2, the solution A is poured into an inner liner of polytetrafluoroethylene for sealing, then the inner liner is arranged in an outer kettle, and the outer kettle is fixed and then placed in a homogeneous phase reactor for hydrothermal reaction.
Preferably, in the step 2, the temperature of the solution A for hydrothermal reaction is controlled within the range of 160-180 ℃, and the reaction time is 5-8 h.
Preferably, in the step 3, the CdS powder, nickel chloride hexahydrate and urea are added into a reaction kettle with a polytetrafluoroethylene lining, deionized water is added, and then stirring is carried out, so as to obtain a yellow-green solution B.
Preferably, in the step 3, the CdS powder, nickel chloride hexahydrate and urea are added into a reaction kettle with a polytetrafluoroethylene lining, and the filling ratio ranges from 20% to 40%.
Preferably, in the step 4, the reaction temperature of the hydrothermal reaction ranges from 120 ℃ to 140 ℃, and the reaction time ranges from 12h to 16 h.
The CdS composite photocatalyst can absorb and utilize solar energy, excite electrons under the illumination condition to transfer the solar energy, and finally convert the solar energy into clean hydrogen energy.
Compared with the prior art, the invention has the following beneficial technical effects:
compared with pure-phase CdS, Ni-CdS has better conductivity, and Ni and CdS are doped, so that the charge transfer rate of CdS is improved, the conductivity is better, the charge transfer rate is higher, the recombination and the photo-corrosion phenomena of electron-hole pairs are inhibited, and the photo-corrosion phenomenon of CdS is inhibited, so that the aim of improving the hydrogen production by photocatalysis of CdS is further fulfilled.
The invention provides a preparation method of a hydrothermally synthesized Ni-doped CdS composite photocatalyst, which is characterized in that Ni and CdS are doped by adopting a hydrothermal method, so that the charge transfer rate of CdS is improved, the photo-corrosion phenomenon of CdS is inhibited, and the aim of improving the hydrogen production by CdS photocatalysis is further fulfilled. Compared with the preparation strategy, the invention adopts a hydrothermal method, and has the characteristics of simple reaction process, low synthesis temperature, no need of large-scale equipment and harsh conditions and the like. The product prepared by the method has uniform chemical composition, high purity and uniform appearance, can show good photochemical performance when being used as a material for producing hydrogen by photolyzing water, and can keep stability for at least 16h under the irradiation of an argon lamp.
Drawings
FIG. 1 is a CdS and Ni-CdS X-ray diffraction analysis chart of example 1 of the present invention;
FIG. 2a is a CdS scanning analysis chart of example 1 according to the present invention;
FIG. 2b is a scanning analysis chart of Ni-CdS in example 1 of the present invention;
FIG. 3a is a hydrogen production rate diagram for CdS, CdS/Pt (1%) and Ni-CdS of example 1 according to the present invention;
FIG. 3b is a cycle diagram of Ni-CdS hydrogen production in example 1 of the present invention.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The invention relates to a Ni-doped CdS composite photocatalyst synthesized by a hydrothermal method and a preparation method thereof, wherein the Ni-doped CdS composite photocatalyst comprises the following steps:
And 3, pouring the solution A into an inner liner of polytetrafluoroethylene for sealing, then placing the inner liner into an outer kettle for fixing, and then placing the inner liner into a homogeneous reactor, wherein the filling ratio is controlled at 60%. The temperature is controlled to be 160-180 ℃, and the reaction time is controlled to be 5-8 h. Then the reaction kettle is naturally cooled to the room temperature.
And 4, after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, pouring out the cooled solution after the reaction, performing suction filtration alternately for three times of water and three times of water, collecting a product, and drying the product for 6-8 hours at the temperature of 60-80 ℃ under a vacuum condition. And pouring the dried sample into a mortar to be ground into a fine powder sample, thus obtaining the CdS material.
And 5, putting 0.06-0.1 g of CdS powder, 0.02-0.06 g of nickel chloride hexahydrate and 0.6-1.0 g of urea into a 100mL of polytetrafluoroethylene-lined high-temperature and high-pressure reaction kettle, adding 20-40 mL of deionized water again, and stirring for 0.5-1 h at the speed of 500-800 r/min in a magnetic stirrer to obtain a yellow-green solution B.
And step 6, then, placing the inner liner in an outer kettle, fixing the inner liner in a homogeneous reactor, controlling the filling ratio to be 20-40%, controlling the temperature to be 120-140 ℃, controlling the reaction time to be 12-16 h, and naturally cooling the reaction kettle to room temperature.
And 7, after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, pouring out the cooled solution after the reaction, performing suction filtration alternately for three times of water and three times of water, collecting a product, and drying the product for 6-8 hours at the temperature of 60-80 ℃ under a vacuum condition. And pouring the dried sample into a mortar and grinding the dried sample into a fine powder sample to obtain the Ni-doped CdS composite photocatalyst material.
Example 1:
1) first, cadmium acetate, thioacetamide and other raw materials were weighed in the following molar ratios.
C4H6CdO4·2H2O：CH3CSNH2＝0.5:0.6
2) 60ml of ethylene diamine and ethylene glycol are added into the prepared materials according to the volume ratio: 1:1 and then stirring for 0.5h at a speed of 500r/min in a magnetic stirrer to obtain a transparent solution A.
3) Pouring the solution A into an inner liner of polytetrafluoroethylene for sealing, then placing the inner liner into an outer kettle for fixing, and then placing the inner liner into a homogeneous reactor, wherein the filling ratio is controlled at 60%. The temperature is controlled at 160 ℃, and the reaction time is controlled at 8 h. Then the reaction kettle is naturally cooled to the room temperature.
4) And after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, pouring out the cooled solution after the reaction, performing suction filtration alternately for three times of water and three times of water, collecting a product, and drying the product for 6 hours at 60 ℃ under a vacuum condition. And pouring the dried sample into a mortar to be ground into a fine powder sample, thus obtaining the CdS material.
5) Then 0.06g CdS powder, 0.02g nickel chloride hexahydrate and 0.6g urea are put into a high-temperature high-pressure reaction kettle with a 100mL polytetrafluoroethylene lining, 20mL deionized water is added again, and then the mixture is stirred in a magnetic stirrer at the speed of 500r/min for 0.5h to obtain a yellow-green solution B.
6) Then the inner liner is arranged in an outer kettle and fixed, and then the inner liner is placed in a homogeneous reactor, the filling ratio is controlled at 20 percent, the temperature is controlled at 120 ℃, the reaction time is controlled at 12h, and the reaction kettle is naturally cooled to the room temperature.
7) And after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, pouring out the cooled solution after the reaction, performing suction filtration alternately for three times of water and three times of water, collecting a product, and drying the product for 6 hours at 60 ℃ under a vacuum condition. And pouring the dried sample into a mortar and grinding the dried sample into a fine powder sample to obtain the Ni-doped CdS composite photocatalyst material.
Example 2:
1) first, cadmium acetate, thioacetamide and other raw materials were weighed in the following molar ratios.
C4H6CdO4·2H2O：CH3CSNH2＝0.6:0.7。
2) 60ml of ethylene diamine and ethylene glycol are added into the prepared materials according to the volume ratio: 2: 1A clear solution A was then obtained after stirring for 1h at a speed of 600r/min with a magnetic stirrer.
3) Pouring the solution A into an inner liner of polytetrafluoroethylene for sealing, then placing the inner liner into an outer kettle for fixing, and then placing the inner liner into a homogeneous reactor, wherein the filling ratio is controlled at 60%. The temperature is controlled at 170 ℃, and the reaction time is controlled at 7 h. Then the reaction kettle is naturally cooled to the room temperature.
4) And after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, pouring out the cooled solution after the reaction, performing suction filtration alternately for three times of water and three times of water, collecting a product, and drying the product at 75 ℃ for 7 hours under a vacuum condition. And pouring the dried sample into a mortar to be ground into a fine powder sample, thus obtaining the CdS material.
5) Then 0.07g CdS powder, 0.03g nickel chloride hexahydrate and 0.7g urea are put into a high-temperature high-pressure reaction kettle with a 100mL polytetrafluoroethylene lining, 30mL deionized water is added again, and then the mixture is stirred in a magnetic stirrer at the speed of 600r/min for 0.5h to obtain a yellow-green solution B.
6) Then the inner liner is arranged in an outer kettle and fixed, and then the inner liner is placed in a homogeneous reactor, the filling ratio is controlled at 30 percent, the temperature is controlled at 120 ℃, the reaction time is controlled at 13h, and the reaction kettle is naturally cooled to the room temperature.
7) And after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, pouring out the cooled solution after the reaction, performing suction filtration alternately for three times of water and three times of water, collecting a product, and drying the product at 60 ℃ for 7 hours under a vacuum condition. And pouring the dried sample into a mortar and grinding the dried sample into a fine powder sample to obtain the Ni-doped CdS composite photocatalyst material.
Example 3:
1) first, cadmium acetate, thioacetamide and other raw materials were weighed in the following molar ratios.
C4H6CdO4·2H2O：CH3CSNH2＝0.7:0.8。
2) 60ml of ethylene diamine and ethylene glycol are added into the prepared materials according to the volume ratio: 3: 1A clear solution A was then obtained after stirring for 1h at a speed of 700r/min with a magnetic stirrer.
3) Pouring the solution A into an inner liner of polytetrafluoroethylene for sealing, then placing the inner liner into an outer kettle for fixing, and then placing the inner liner into a homogeneous reactor, wherein the filling ratio is controlled at 60%. The temperature is controlled at 180 ℃, and the reaction time is controlled at 6 h. Then the reaction kettle is naturally cooled to the room temperature.
4) And after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, pouring out the cooled solution after the reaction, performing suction filtration alternately for three times of water and three times of water, collecting a product, and drying the product for 6 hours at 80 ℃ under a vacuum condition. And pouring the dried sample into a mortar to be ground into a fine powder sample, thus obtaining the CdS material.
5) And then 0.08g of CdS powder, 0.04g of nickel chloride hexahydrate and 0.8g of urea are put into a high-temperature and high-pressure reaction kettle with a 100mL polytetrafluoroethylene lining, 35mL of deionized water is added again, and then the mixture is stirred in a magnetic stirrer at the speed of 700r/min for 1 hour to obtain a yellow-green solution B.
6) Then the inner liner is arranged in an outer kettle and fixed, and then the inner liner is placed in a homogeneous reactor, the filling ratio is controlled at 35%, the temperature is controlled at 130 ℃, the reaction time is controlled at 14h, and the reaction kettle is naturally cooled to the room temperature.
6) And after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, pouring out the cooled solution after the reaction, performing suction filtration alternately for three times of water and three times of water, collecting a product, and drying the product at 70 ℃ for 7 hours under a vacuum condition. And pouring the dried sample into a mortar and grinding the dried sample into a fine powder sample to obtain the Ni-doped CdS composite photocatalyst material.
Example 4:
1) first, cadmium acetate, thioacetamide and other raw materials were weighed in the following molar ratios.
C4H6CdO4·2H2O：CH3CSNH2＝0.8:0.9。
2) 60ml of ethylene diamine and ethylene glycol are added into the prepared materials according to the volume ratio: 4:1 then a clear solution A was obtained after stirring for 2h at a speed of 800r/min with a magnetic stirrer.
3) Pouring the solution A into an inner liner of polytetrafluoroethylene for sealing, then placing the inner liner into an outer kettle for fixing, and then placing the inner liner into a homogeneous reactor, wherein the filling ratio is controlled at 60%. The temperature is controlled at 180 ℃, and the reaction time is controlled at 5 h. Then the reaction kettle is naturally cooled to the room temperature.
4) And after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, pouring out the cooled solution after the reaction, performing suction filtration alternately for three times of water and three times of water, collecting a product, and drying the product for 6 hours at 80 ℃ under a vacuum condition. And pouring the dried sample into a mortar to be ground into a fine powder sample, thus obtaining the CdS material.
5) Then 0.09g of CdS powder, 0.05g of nickel chloride hexahydrate and 0.9g of urea are put into a high-temperature and high-pressure reaction kettle with a 100mL polytetrafluoroethylene lining, 40mL of deionized water is added again, and then the mixture is stirred in a magnetic stirrer at the speed of 800r/min for 1 hour to obtain a yellow-green solution B.
6) Then the inner liner is arranged in an outer kettle and fixed, and then the inner liner is placed in a homogeneous reactor, the filling ratio is controlled at 40 percent, the temperature is controlled at 140 ℃, the reaction time is controlled at 15h, and the reaction kettle is naturally cooled to the room temperature.
7) And after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, pouring out the cooled solution after the reaction, performing suction filtration alternately for three times of water and three times of water, collecting a product, and drying the product for 6 hours at 80 ℃ under a vacuum condition. And pouring the dried sample into a mortar and grinding the dried sample into a fine powder sample to obtain the Ni-doped CdS composite photocatalyst material.
Example 5:
1) first, cadmium acetate, thioacetamide and other raw materials were weighed in the following molar ratios.
C4H6CdO4·2H2O：CH3CSNH2＝0.9:1.0.
2) 60ml of ethylene diamine and ethylene glycol are added into the prepared materials according to the volume ratio: 5:1 then a clear solution A was obtained after stirring for 2h at a speed of 800r/min with a magnetic stirrer.
3) Pouring the solution A into an inner liner of polytetrafluoroethylene for sealing, then placing the inner liner into an outer kettle for fixing, and then placing the inner liner into a homogeneous reactor, wherein the filling ratio is controlled at 60%. The temperature is controlled at 180 ℃, and the reaction time is controlled at 8 h. Then the reaction kettle is naturally cooled to the room temperature.
4) And after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, pouring out the cooled solution after the reaction, performing suction filtration alternately for three times of water and three times of water, collecting a product, and drying the product for 8 hours at 80 ℃ under a vacuum condition. And pouring the dried sample into a mortar to be ground into a fine powder sample, thus obtaining the CdS material.
5) Then 0.1g CdS powder, 0.06g nickel chloride hexahydrate and 1.0g urea are put into a high-temperature high-pressure reaction kettle with a 100mL polytetrafluoroethylene lining, 40mL deionized water is added again, and then the mixture is stirred for 1 hour in a magnetic stirrer at the speed of 800r/min to obtain a yellow-green solution B.
6) Then the inner liner is arranged in an outer kettle and fixed, and then the inner liner is placed in a homogeneous reactor, the filling ratio is controlled at 40 percent, the temperature is controlled at 140 ℃, the reaction time is controlled at 16h, and the reaction kettle is naturally cooled to the room temperature.
7) And after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, pouring out the cooled solution after the reaction, performing suction filtration alternately for three times of water and three times of water, collecting a product, and drying the product for 8 hours at 80 ℃ under a vacuum condition. And pouring the dried sample into a mortar and grinding the dried sample into a fine powder sample to obtain the Ni-doped CdS composite photocatalyst material.
Claims (10)
1. The composite photocatalyst for hydrothermally synthesizing Ni-doped CdS is characterized by comprising the following components in parts by weight (1-2) to (0.4-1): (10-20) CdS powder, nickel chloride hexahydrate and urea.
2. The hydrothermally synthesized Ni-doped CdS composite photocatalyst as claimed in claim 1, wherein the hydrothermally synthesized Ni-doped CdS composite photocatalyst is synthesized by a hydrothermal reaction.
3. A preparation method of a Ni-doped CdS composite photocatalyst by hydrothermal synthesis is characterized by comprising the following processes,
step 1, weighing cadmium acetate and thioacetamide according to the ratio of (0.5-0.8) to (0.6-1.2), adding ethylenediamine and ethylene glycol according to the ratio of (1-4) to 1, and stirring to form a solution A;
step 2, carrying out hydrothermal reaction on the solution A, and filtering to obtain CdS powder;
step 3, mixing the components in the ratio of (1-2) to (0.4-1): (10-20) adding the CdS powder, nickel chloride hexahydrate and urea into deionized water, and stirring to obtain a solution B;
and 4, carrying out hydrothermal reaction on the solution B, filtering and drying to obtain the Ni-doped CdS composite photocatalyst material.
4. The method for preparing a hydrothermally synthesized Ni-doped CdS composite photocatalyst according to claim 3, wherein in the step 1, a magnetic stirrer is used for stirring at a speed of 500 r/min-800 r/min for 0.5-2 h to obtain a transparent solution A.
5. The method for preparing a hydrothermally synthesized Ni-doped CdS composite photocatalyst according to claim 3, wherein in step 2, the solution A is poured into an inner liner of polytetrafluoroethylene for sealing, then the inner liner is arranged in an outer kettle, and the outer kettle is fixed and then placed in a homogeneous phase reactor for hydrothermal reaction.
6. The preparation method of the hydrothermally synthesized Ni-doped CdS composite photocatalyst according to claim 3, wherein in the step 2, the temperature of the solution A for the hydrothermal reaction is controlled within a range of 160-180 ℃ and the reaction time is 5-8 h.
7. The method for preparing a hydrothermally synthesized Ni-doped CdS composite photocatalyst according to claim 3, wherein in step 3, CdS powder, nickel chloride hexahydrate and urea are added into a reaction kettle with a polytetrafluoroethylene lining, and are stirred after deionized water is added, so that a yellow-green solution B is obtained.
8. The preparation method of the Ni-doped CdS composite photocatalyst through hydrothermal synthesis according to claim 3, wherein in the step 3, CdS powder, nickel chloride hexahydrate and urea are added into a reaction kettle with a polytetrafluoroethylene lining, and the filling ratio ranges from 20% to 40%.
9. The preparation method of the hydrothermally synthesized Ni-doped CdS composite photocatalyst according to claim 3, wherein in step 4, the reaction temperature of the hydrothermal reaction is 120-140 ℃, and the reaction time is 12-16 h.
10. An application of a hydrothermally synthesized Ni-doped CdS composite photocatalyst is characterized in that the CdS composite photocatalyst as claimed in claims 1-2 can absorb and utilize solar energy, excite electrons under the illumination condition to transfer the electrons, and finally convert the solar energy into clean hydrogen energy.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114950487A (en) * | 2022-06-01 | 2022-08-30 | 陕西科技大学 | Polished glutinous rice strip CdS/Ni-CdVO 6 Composite photocatalyst and preparation method and application thereof |
| CN115301194A (en) * | 2022-07-22 | 2022-11-08 | 南开大学 | Nano composite material and preparation method and application thereof |
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| CN115845878A (en) * | 2022-12-31 | 2023-03-28 | 吉林化工学院 | Ni/CdS catalyst and preparation method and application thereof |
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- 2021-12-27 CN CN202111620458.3A patent/CN114272939A/en not_active Withdrawn
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| CN114950487A (en) * | 2022-06-01 | 2022-08-30 | 陕西科技大学 | Polished glutinous rice strip CdS/Ni-CdVO 6 Composite photocatalyst and preparation method and application thereof |
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| CN115301194A (en) * | 2022-07-22 | 2022-11-08 | 南开大学 | Nano composite material and preparation method and application thereof |
| CN115779932A (en) * | 2022-11-01 | 2023-03-14 | 陕西科技大学 | V-CdS/NiS 2 Preparation method of composite photocatalyst |
| CN115779932B (en) * | 2022-11-01 | 2024-04-02 | 陕西科技大学 | V-CdS/NiS 2 Preparation method of composite photocatalyst |
| CN115845878A (en) * | 2022-12-31 | 2023-03-28 | 吉林化工学院 | Ni/CdS catalyst and preparation method and application thereof |
| CN115845878B (en) * | 2022-12-31 | 2024-05-07 | 吉林化工学院 | Ni/CdS catalyst and preparation method and application thereof |
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