CN115212909B - Cauliflower-shaped CdS/C 3 N 4 Hydrothermal synthesis method of composite material and application thereof - Google Patents

Cauliflower-shaped CdS/C 3 N 4 Hydrothermal synthesis method of composite material and application thereof Download PDF

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CN115212909B
CN115212909B CN202210823188.4A CN202210823188A CN115212909B CN 115212909 B CN115212909 B CN 115212909B CN 202210823188 A CN202210823188 A CN 202210823188A CN 115212909 B CN115212909 B CN 115212909B
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兰东辉
章步鑫
易兵
肖广
杨秀康
沈静
伍水生
杜紫妍
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Hunan Institute of Engineering
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Abstract

The invention discloses a cauliflower-shaped CdS/C 3 N 4 The hydrothermal synthesis method and application of the composite material comprise the following steps: (1) Will g-C 3 N 4 Adding the soluble cadmium salt into water, and performing ultrasonic grinding to obtain a mixed solution A; vitamin B 1 Dissolving hydrochloride and hexamethylenetetramine in water to obtain a solution B, and then adding the solution B into the solution A under stirring to obtain a mixed solution C; (3) Performing hydrothermal treatment on the mixed solution C to obtain cauliflower-shaped CdS/C 3 N 4 A composite material. The invention uses vitamin B 1 The hydrochloride is used as a sulfur source and a surfactant, so that CdS forms cauliflower-shaped nano particles with smaller size, which is beneficial to g-C 3 N 4 And the S-schema heterojunction is constructed by compounding with CdS, so that the separation of photo-generated electrons and holes is promoted, the utilization rate of visible light is improved, cr (VI) can be efficiently catalyzed and reduced under the condition of visible light, and the concentration of the Cr (VI) is reduced to be below 0.5 mg/L.

Description

Cauliflower-shaped CdS/C 3 N 4 Hydrothermal synthesis method of composite material and application thereof
Technical Field
The invention belongs to the technical field of material preparation and environmental protection, and in particular relates to a cauliflower-shaped CdS/C 3 N 4 A hydrothermal synthesis method of composite material and application thereof in visible light catalytic reduction of potassium dichromate.
Background
Chromium is a common heavy metal pollutant in industrial wastewater of electroplating, metallurgy, printing and dyeing and the like, and the main existing forms of chromium in the nature comprise two oxidation states of chromium (VI) and chromium (III). Among them, cr (VI) concentration is too high, is toxic to most organisms, is carcinogenic to animals and humans, causes irritation, and can be enriched by bio-chain action. Therefore, cr (VI) must be removed from the chromium (VI) containing wastewater before it is discharged into the environment.
Among the reported methods, the reduction of hexavalent chromium to trivalent chromium by semiconductor-based photocatalytic methods has been the focus of much research. The photocatalytic reduction method for reducing hexavalent chromium is one of strategies for effectively repairing polluted wastewater due to high efficiency, environmental protection and low cost, and is also one of the preferred methods for reducing hexavalent chromium.
Many photocatalysts have been developed for the remediation of industrial effluent environmental pollutants such as titanium dioxide, bismuth sulfide, zinc oxide, graphite nitride and cadmium sulfide. CdS was introduced as a suitable visible light driven photocatalyst because its bandgap is relatively narrow, about 2.4eV, and the suitable band edge position corresponds well to the solar spectrum. However, the rapid recombination of electron-hole pairs, photo-etching, and low surface reaction efficiency of CdS materials have prevented their use as an effective photocatalyst.
In order to improve the photocatalytic efficiency of CdS nanostructures, many studies have been conducted to control the particle size and morphology of CdS nanostructures, since these parameters directly affect the surface area, light absorption capacity and carrier dynamics of the catalyst. The nano-structure of the CdS prepared at present is various, such as nanospheres, nanorods, nanosheets, nanobelts, nanotubes, layered nano-structures, petal-shaped nano-structures, hollow nano-structures and the like.
Disclosure of Invention
Aiming at the problems of fast recombination of CdS electron-hole pairs, serious photo-corrosion and low surface reaction efficiency, the invention aims to provide a cauliflower-shaped CdS/C 3 N 4 Hydrothermal synthesis method of nanocomposite material with vitamin B 1 Hydrochloride as sulfur source and surfactant, cd 2+ With vitamin B 1 The hydrochloride salt provides a sulfur source to produce CdS, and the CdS is reacted with g-C 3 N 4 In-situ composite construction of heterojunction, after the composition, cdS forms smaller cauliflower-shaped nano particles, and the size is increasedThe surface area promotes the separation of photo-generated electrons and holes, improves the utilization rate of visible light, and can efficiently catalyze and reduce Cr (VI) under the condition of visible light, so that the concentration of the Cr (VI) is reduced to below 0.5mg/L, and the emission standard is reached.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
cauliflower-shaped CdS/C 3 N 4 The hydrothermal synthesis method of the composite material comprises the following steps:
(1) Will g-C 3 N 4 Adding the soluble cadmium salt into water, and performing ultrasonic grinding to obtain a mixed solution A; vitamin B 1 Dissolving hydrochloride and hexamethylenetetramine in water to obtain a solution B, and then adding the solution B into the solution A under stirring to obtain a mixed solution C;
(2) Carrying out hydrothermal treatment on the mixed solution C, and carrying out solid-liquid separation, washing and drying to obtain the CdS/C 3 N 4 A composite material.
g-C of the invention 3 N 4 Can be prepared by the prior conventional method, for example, one or more of urea, melamine and thiourea are used as precursors, and the g-C can be obtained by calcining 3 N 4 And will not be described in detail herein.
Preferably, in the step (1), the soluble cadmium salt is selected from one or more of cadmium nitrate, cadmium sulfate and cadmium acetate.
Preferably, in step (1), the soluble cadmium salt is mixed with g-C 3 N 4 The mass ratio of (2) is 1-10:1.
Preferably, in the step (1), the concentration of the soluble cadmium salt in the mixed solution A is 0.02-0.2 mol/L.
Preferably, in step (1), the soluble cadmium salt, vitamin B 1 The mol ratio of the hydrochloride to the hexamethylenetetramine is 1:1-5:1-4.
Preferably, in the step (1), vitamin B is contained in the mixed solution B 1 The concentration of the hydrochloride is 0.1 to 0.3mol/L.
Preferably, in the step (2), the temperature of the hydrothermal treatment is 100-180 ℃ and the time is 1-24 hours.
The invention also providesThe cauliflower-like CdS/C 3 N 4 The application of the composite material is that the composite material is used as a photocatalyst for reducing potassium dichromate under visible light;
the method comprises the following specific steps: at room temperature, cauliflower-like CdS/C 3 N 4 The composite material is added into water with the potassium dichromate concentration of 10-250 mg/L and reacts for 0.1-12 h.
Preferably, the cauliflower-like CdS/C 3 N 4 The volume ratio of the mass of the composite material to the potassium dichromate solution is 1 mg:0.5-2 mL.
The invention utilizes vitamin B 1 As sulfur source and surfactant, hexamethylenetetramine is used as cadmium ion complexing agent and alkali to promote vitamin B 1 The hydrochloride salt released sulfur in g-C 3 N 4 Is a carrier, cd 2+ With vitamin B 1 The hydrochloride provides a sulfur source to generate CdS, and g-C 3 N 4 The heterojunction is built by compounding, so that smaller cauliflower-shaped nano particles are formed by CdS, the surface area is increased, the separation of photo-generated electrons and holes is promoted, and the utilization rate of visible light is improved. Under the condition of visible light, the method can efficiently catalyze and reduce Cr (VI) to ensure that the concentration of the Cr (VI) is reduced to be below 0.5mg/L and reaches the emission standard.
Compared with the prior art, the invention has the advantages that:
1. vitamin B in the invention 1 Hydrochloride is used as a sulfur source and a surfactant; hexamethylene tetramine is used as a cadmium ion complexing agent and also used as alkali to promote vitamin B 1 The hydrochloride is explained to release sulfur, and the sulfur and soluble cadmium salt are controllably synthesized into CdS.
2. The invention adopts the hydrothermal preparation technology to controllably synthesize CdS/C 3 N 4 The composite material forms a cauliflower-shaped composite material, the particle size is obviously reduced, and the precise construction of the high-efficiency visible light photocatalyst is facilitated.
3. CdS/C prepared by the invention 3 N 4 The composite material has a nano-size structure, and can efficiently reduce Cr (VI) in water under visible light, so that the concentration of the Cr (VI) is reduced to below 0.5 mg/L.
Drawings
FIG. 1 is an XRD spectrum of the material prepared in example 1 and comparative example 1;
fig. 2 is an SEM image of the material prepared in example 1.
Fig. 3 is an SEM image of the material prepared in comparative example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
6.9mmol of cadmium nitrate is dissolved in 50mL of water, and 0.2gg-C is added 3 N 4 Ultrasonic dispersion for 0.5h by a cell pulverizer to obtain a mixed solution A, and dropwise adding 25mL of vitamin B containing 7.4mmol into the mixed solution A 1 The aqueous solution B of hydrochloride and 14mmol of hexamethylenetetramine is stirred uniformly, transferred to a hydrothermal kettle, sealed and subjected to hydrothermal treatment at 100 ℃ for 24 hours to obtain a mixed solution C, and the mixed solution C is washed and dried to obtain the dark yellow solid CdS/C 3 N 4 A composite material.
Example 2
2.5mmol of cadmium sulfate was dissolved in 40mL of water and 0.1333gg-C was added 3 N 4 Ultrasonic dispersing for 0.5h by a cell pulverizer to obtain a mixed solution A, and dropwise adding 30mL of vitamin B containing 3mmol into the mixed solution A 1 The hydrochloride and 10mmol of hexamethylene tetramine water solution B are stirred uniformly, transferred to a hydrothermal kettle, sealed and subjected to hydrothermal treatment at 160 ℃ for 24 hours to obtain a mixed solution C, and the mixed solution C is washed and dried to obtain dark yellow solid CdS/C 3 N 4 A composite material.
Example 3
2.5mmol of cadmium nitrate was dissolved in 30mL of water and 0.2gg-C was added 3 N 4 Ultrasonic dispersing for 0.5h by a cell pulverizer to obtain a mixed solution A, and dropwise adding 20mL of vitamin B containing 3mmol into the mixed solution A 1 The aqueous solution B of hydrochloride and 5mmol of hexamethylenetetramine is stirred uniformly, transferred to a hydrothermal kettle, sealed and subjected to hydrothermal treatment at 160 ℃ for 24 hours to obtain a mixed solution C, and the mixed solution C is washed and dried to obtain the dark yellow solid CdS-C 3 N 4 A composite material.
Example 4
2.5mmol of cadmium nitrate was dissolved in 50mL of water and 0.2667gg-C was added 3 N 4 Ultrasonic dispersing for 0.5h by a cell pulverizer to obtain a mixed solution A, and dropwise adding 30mL of vitamin B containing 3mmol into the mixed solution A 1 The hydrochloride and 5mmol of hexamethylene tetramine water solution B are stirred uniformly, transferred to a hydrothermal kettle, sealed, subjected to hydrothermal treatment at 180 ℃ for 1h to obtain a mixed solution C, washed and dried to obtain dark yellow solid CdS/C 3 N 4 A composite material.
Comparative example 1
Weighing 6.9mmol of cadmium nitrate, dissolving in 50mL of water, performing ultrasonic dispersion for 0.5h by a cell pulverizer, and dropwise adding 25mL of solution containing 7.4mmol of vitamin B 1 And (3) uniformly stirring the aqueous solution of hydrochloride and 14mmol of hexamethylenetetramine, transferring to a hydrothermal kettle, sealing, performing hydrothermal treatment at 100 ℃ for 24 hours, and washing and drying to obtain the dark yellow solid CdS.
Comparative example 2
15g of urea is weighed and added into a glass dish, and the tinfoil paper is sealed and then placed into a muffle furnace for heat treatment. Heating from room temperature to 250deg.C at a rate of 2deg.C/min, maintaining for 2 hr, heating to 530 deg.C at a rate of 5deg.C/min, maintaining for 2 hr, cooling to room temperature to obtain pale yellow solid, washing with acid, washing with water to neutrality, and oven drying to obtain pale yellow solid g-C 3 N 4 。
Comparative example 3
Weighing 2.5mmol of cadmium nitrate, dissolving in 50mL of water, adding 0.2gg-C 3 N 4 After the cell grinder is subjected to ultrasonic dispersion for 0.5h, 20mL of aqueous solution containing 3mmol of sodium sulfide and 5mmol of hexamethylenetetramine is dropwise added, after uniform stirring, the mixture is transferred to a hydrothermal kettle to be sealed, and then is subjected to hydrothermal treatment at 160 ℃ for 24h, and after washing and drying, the dark yellow solid CdS/C is obtained 3 N 4 A composite material.
Comparative example 4
6.9mmol of cadmium nitrate is dissolved in 50mL of water, and 0.2gg-C is added 3 N 4 Ultrasonic dispersion for 0.5h by a cell pulverizer to obtain a mixed solution A, and dropwise adding 25mL of vitamin B containing 7.4mmol into the mixed solution A 1 Hydrochloric acidThe aqueous solution B of salt is stirred uniformly, transferred to a hydrothermal kettle to be sealed and subjected to hydrothermal treatment at 100 ℃ for 24 hours to obtain a mixed solution C, and the mixed solution C is washed and dried to almost obtain no CdS product which is only a light yellow solid C 3 N 4 。
Reduction of potassium dichromate:
at room temperature, 20mg of the materials prepared in examples 1-4 and comparative examples 1-3 were added into 20mL of potassium dichromate aqueous solution with a concentration of 10-250 mg/L, and subjected to light-shielding ultrasonic dispersion for 15min, dark reaction for 30min, a xenon lamp light source was turned on, the catalyst was removed by filtration after 2h of reaction, the residual Cr (VI) concentration was detected, and the reduction rate was calculated as shown in Table 1:
TABLE 1 data sheet for reduction rate of potassium dichromate
Figure BDA0003745234900000051

Claims (8)

1. Cauliflower-shaped CdS/C 3 N 4 The hydrothermal synthesis method of the composite material is characterized by comprising the following steps of:
(1) Will g-C 3 N 4 Adding the soluble cadmium salt into water, and performing ultrasonic grinding to obtain a mixed solution A; vitamin B 1 Dissolving hydrochloride and hexamethylenetetramine in water to obtain a solution B, and then adding the solution B into the solution A under stirring to obtain a mixed solution C;
(2) Carrying out hydrothermal treatment on the mixed solution C, and carrying out solid-liquid separation, washing and drying to obtain the CdS/C 3 N 4 A composite material;
the temperature of the hydrothermal treatment is 100-180 DEG o And C, the time is 1-24 h.
2. The hydrothermal synthesis method according to claim 1, wherein: in the step (1), the soluble cadmium salt is one or more selected from cadmium nitrate, cadmium sulfate and cadmium acetate.
3. The hydrothermal synthesis method according to claim 1, wherein: in the step (1), the step of (a),the soluble cadmium salt and g-C 3 N 4 The mass ratio of (2) is 1-10:1.
4. The hydrothermal synthesis method according to claim 1, wherein: in the step (1), the concentration of the soluble cadmium salt in the mixed solution A is 0.02-0.2 mol/L.
5. The hydrothermal synthesis method according to claim 1, wherein: in step (1), the soluble cadmium salt and vitamin B 1 The molar ratio of the hydrochloride to the hexamethylenetetramine is 1:1-5:1-4.
6. The hydrothermal synthesis method according to claim 1, wherein: in the step (1), vitamin B in the mixed solution B 1 The concentration of the hydrochloride is 0.1-0.3 mol/L.
7. The cauliflower-like CdS/C synthesized by the hydrothermal synthesis method of any one of claims 1 to 6 3 N 4 The application of the composite material is characterized in that: the catalyst is used as a photocatalyst for reducing potassium dichromate under visible light;
the method comprises the following specific steps: at room temperature, cauliflower-like CdS/C 3 N 4 The composite material is added into water with the potassium dichromate concentration of 10-250 mg/L, and the reaction is carried out for 0.1-12 h.
8. The cauliflower-like CdS/C according to claim 7 3 N 4 The application of the composite material is characterized in that: the cauliflower-shaped CdS/C 3 N 4 The ratio of the mass of the composite material to the volume of the potassium dichromate solution is 1 mg:0.5-2 mL.
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