CN109499594A - A kind of CdIn2S4 nanometers of octahedra modification Ta3N5The preparation method of nucleocapsid composite photo-catalyst - Google Patents

A kind of CdIn2S4 nanometers of octahedra modification Ta3N5The preparation method of nucleocapsid composite photo-catalyst Download PDF

Info

Publication number
CN109499594A
CN109499594A CN201811319448.4A CN201811319448A CN109499594A CN 109499594 A CN109499594 A CN 109499594A CN 201811319448 A CN201811319448 A CN 201811319448A CN 109499594 A CN109499594 A CN 109499594A
Authority
CN
China
Prior art keywords
cdin
nano
core
modified
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201811319448.4A
Other languages
Chinese (zh)
Other versions
CN109499594B (en
Inventor
彭志远
王旭乾
曹清源
蒋银花
张申
张文莉
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Chongqing Science City Intellectual Property Operation Center Co ltd
Xi'an Meinan Biotechnology Co ltd
Original Assignee
Jiangsu University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangsu University filed Critical Jiangsu University
Priority to CN201811319448.4A priority Critical patent/CN109499594B/en
Publication of CN109499594A publication Critical patent/CN109499594A/en
Application granted granted Critical
Publication of CN109499594B publication Critical patent/CN109499594B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • B01J27/24—Nitrogen compounds
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
    • B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/396—Distribution of the active metal ingredient
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/308—Dyes; Colorants; Fluorescent agents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/34—Organic compounds containing oxygen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/38—Organic compounds containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/40—Organic compounds containing sulfur
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/10—Photocatalysts

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Catalysts (AREA)

Abstract

本发明属于无机纳米复合材料的制备及环境治理领域，具体公开了具有可见光活性的CdIn2S4纳米八面体修饰Ta3N5核壳复合光催化剂的制备方法。通过原位水热法制备不同比例的CdIn2S4纳米八面体修饰Ta3N5核壳复合光催化剂。结合两种材料的优势及匹配的能带结构，实现光生电子在不同能级间的高效转移，提高光生载流子的分离效率，进而实现可见光下高效降解染料甲基橙。本发明具有制备原料环保，方法简单，杂化反应条件温和，周期短和成本低等优点。本发明首次报道了这种核壳复合光催化剂，CdIn2S4纳米八面体修饰Ta3N5核壳结构表现出优良的光催化降解活性，在处理染料废水方面具有重要的应用前景。

The invention belongs to the field of preparation and environmental treatment of inorganic nano composite materials, and specifically discloses a preparation method of a CdIn 2 S 4 nano-octahedron modified Ta 3 N 5 core-shell composite photocatalyst with visible light activity. Different ratios of CdIn2S4 nano - octahedron-modified Ta3N5 core - shell composite photocatalysts were prepared by in situ hydrothermal method. Combining the advantages of the two materials and matching energy band structures, the efficient transfer of photogenerated electrons between different energy levels is realized, the separation efficiency of photogenerated carriers is improved, and the dye methyl orange is efficiently degraded under visible light. The invention has the advantages of environment-friendly preparation of raw materials, simple method, mild hybridization reaction conditions, short period and low cost. This core-shell composite photocatalyst is reported for the first time in the present invention. The Ta 3 N 5 core-shell structure modified by CdIn 2 S 4 nano-octahedron shows excellent photocatalytic degradation activity and has important application prospects in the treatment of dye wastewater.

Description

A kind of CdIn2S4The octahedra modification Ta of nanometer3N5The preparation of nucleocapsid composite photo-catalyst Method
Technical field
The invention belongs to field of inorganic nano material, are related to a kind of CdIn2S4The octahedra modification Ta of nanometer3N5Nucleocapsid is compound The preparation method of photochemical catalyst and its application in field of environmental improvement.
Background technique
Since 21 century, with industrialized fast development, world population persistently increases, and water pollution problem has become For one of the key factor for restricting modernization industry development and human survival；And the photocatalytic oxidation degradation based on semiconductor material Technology due to it is its efficiently, green, it is without secondary pollution the advantages that be considered as that solve Different Waters organic compound dirty One of the desirable route of dye problem.However, the forbidden band of most semiconductor light-catalyst is wider at present, can only be swashed by ultraviolet light Hair, limits its utilization to sunlight；Meanwhile higher photo-generated carrier recombination rate results in material entirety photo-quantum efficiency It is lower；Thus, exploitation efficient visible light responsive photocatalyst becomes the necessity of photocatalysis technology development.
In recent years, with the development of functional material, ternary metal sulfide has unique photoelectric property and urges as a kind of The novel photocatalyst for changing performance is greatly paid close attention to, CdIn2S4It is that one kind belongs to as wherein most representative one kind The cubic spinel type semiconductor of Fd3m space group.Body phase CdIn2S4Forbidden bandwidth be 2.1-2.6eV, have it is extremely strong visible Absorbing properties；Simultaneously as it is with good physicochemical stability, it is considered to be the novel light of one kind with development potential is urged Change material.However, higher photo-generate electron-hole combined efficiency has contained it in the fast development of photocatalysis field.Through studying It was found that it is that a kind of very good solution is known that it is carried out with other bulk semiconductors to compound building hybrid heterojunctions.
The Ta-N key as contained in structure and electric conductivity similar with noble metal, make Ta3N5Has excellent thermostabilization Property, mechanical strength, electric conductivity and catalytic performance；Simultaneously because its forbidden bandwidth is relatively narrow (2.1eV), chemical stability is good, There is stronger absorbability in visible light region, it is considered to be a kind of ideal visible light catalyst.Thus, in conjunction with above-mentioned two The advantage and matched band structure of kind material, on the one hand, CdIn can be widened2S4The light abstraction width of material improves quantum and produces Rate；On the other hand have benefited from matched band gap building hybrid heterojunctions, realize efficient transfer of the light induced electron between different energy levels, The separative efficiency of photo-generated carrier is improved, to greatly improve the photocatalytic activity of material.So the present invention provides one kind CdIn2S4The octahedra modification Ta of nanometer3N5The preparation method of nucleocapsid composite photo-catalyst, and study its catalysis under visible light Efficiency.By verification, there is no about CdIn2S4Nanometer octahedron and Ta3N5The report of hybrid, therefore CdIn2S4Nanometer octahedral Body modifies Ta3N5Nucleocapsid compound is a kind of novel photochemical catalyst.
Summary of the invention
In order to widen spectral absorption range, photocatalysis quantum efficiency is improved, the object of the present invention is to provide a kind of CdIn2S4 The octahedra modification Ta of nanometer3N5The preparation method of nucleocapsid composite photo-catalyst；This method prepares CdIn by in-situ method2S4Nanometer Octahedron modification Ta3N5Nucleocapsid composite photo-catalyst, the catalyst can be used under visible light methyl orange of degrading, specific steps It is as follows:
(1) four water cadmium nitrates, nitric hydrate indium and thioacetamide is successively weighed according to certain molar ratio to be added to In the ethanol water of certain volume, stirring 20min forms colourless transparent solution；
(2) Ta of certain mass is weighed3N5Stirring is continued thereafter in the clear solution that nanoparticle is added in step (1) 10-30min, then by uniformly mixed suspension ultrasonic disperse 10-40min to get finely dispersed Ta3N5Nanoparticle mixing Liquid；
(3) by finely dispersed Ta made from step (2)3N5Nano particle mixed liquor, which is transferred in reaction kettle, reacts one section Time is cooled to room temperature after reaction, obtained product secondary deionized water and dehydrated alcohol is washed for several times, very Sky is dry, obtains CdIn2S4The Ta of the octahedra modification of nanometer3N5Nucleocapsid composite photo-catalyst.
In step (1), a mM ratio for four water cadmium nitrates, nitric hydrate indium and thioacetamide is (0.1-4): (0.2-8):(0.8-32)；The amount ratio of four water cadmium nitrates and ethanol water is 0.1-4mmol:10-60mL；Ethanol water In, the volume ratio of dehydrated alcohol and deionized water is 1:0.5-1.
In step (2), Ta3N5The particle size range of nanoparticle is in 300-600nm.
In step (3), reaction temperature is controlled at 160-220 DEG C, and the reaction time is in 8-36h.
CdIn of the present invention2S4The octahedra modification Ta of nanometer3N5In nucleocapsid composite photo-catalyst, CdIn2S4Nanometer eight The mass fraction of face body is in 50-95%, CdIn2S4The octahedral side length of nanometer is in 50-80nm.
A kind of CdIn of the present invention2S4The octahedra modification Ta of nanometer3N5The application of nucleocapsid composite photo-catalyst, the complex light Catalyst can be used for catalyzing oxidizing degrading methyl orange under visible light.
CdIn produced by the present invention2S4The octahedra modification Ta of nanometer3N5It nucleocapsid composite photo-catalyst and its urges under visible light The bring for changing degradation of dye methyl orange has the technical effect that
(1) present invention prepares CdIn for the first time2S4The octahedra modification Ta of nanometer3N5Nucleocapsid composite photo-catalyst, raw materials used peace Completely without pollution, preparation method is simple, and reaction condition is mild, and reaction step is few, easy to operate, and short preparation period is at low cost, favorably In industrialized production；
(2) CdIn prepared by the present invention2S4The octahedra modification Ta of nanometer3N5Nucleocapsid composite photo-catalyst can with excellent The quantum yield of light-exposed response performance, good photostability and brilliance；Meanwhile having benefited from the matched band gap building of the two Hybrid heterojunctions effectively improve the separative efficiency of photo-generated carrier, it is suppressed that photo-generate electron-hole it is compound, thus real The very big leap of existing photocatalysis quantum efficiency.
(3) more single CdIn2S4For the octahedra catalytic effect of nanometer, CdIn2S4The Ta of the octahedra modification of nanometer3N5It is multiple Light combination catalyst shows fabulous photocatalytic activity, realizes compound efficient degradation methyl orange under visible light, has fabulous Application prospect.
Detailed description of the invention
Fig. 1: by CdIn made from example 22S4The octahedra modification Ta of nanometer3N5The SEM of nucleocapsid composite photo-catalyst schemes；
Fig. 2: by CdIn made from example 62S4The octahedra modification Ta of nanometer3N5The TEM of nucleocapsid composite photo-catalyst schemes；
Fig. 3: by CdIn made from example 52S4The octahedra modification Ta of nanometer3N5Outside the solid violet of nucleocapsid composite photo-catalyst- Visible light spectrogram；
Fig. 4: by CdIn made from example 42S4The octahedra modification Ta of nanometer3N5The PL of nucleocapsid composite photo-catalyst schemes.
Specific embodiment
Present invention will be further explained with reference to the attached drawings and specific examples, but protection scope of the present invention is simultaneously It is without being limited thereto.
Degradation experiment carries out in DW-03 type photochemical reactor, using the xenon lamp of 250W as analog solar light source, with filter Mating plate filters ultraviolet light, evaluates CdIn under visible light2S4The Ta of the octahedra modification of nanometer3N5Nucleocapsid composite photo-catalyst is to dirt Contaminate the degradation efficiency of object.Specific step are as follows: the methyl orange solution (MO) of 70mL (10mg/L) is added in reactor and is surveyed Its fixed initial value, is then added the composite photo-catalyst of 20mg, and turn on light illumination 210min, and during which every 30min takes a sample, centrifugation Supernatant is taken after separation, measures the extinction of supernatant in the maximum absorption wave strong point of pollutant with ultraviolet-visible spectrophotometer Degree.According to the absorbance before and after illumination, to calculate degradation rate η=(C of methyl orange solution0-Ct)/C0× 100%, C in formula0For The absorbance of sample, C when illumination just startstFor the absorbance of sample after illumination 3.5h.
Example 1:
(1) four water cadmium nitrates, nitric hydrate indium and thioacetamide are successively weighed according to 0.1:0.2:0.8 mMs of ratio It is added in the ethanol water of 10mL, wherein the volume ratio of dehydrated alcohol and deionized water is 1:0.5, and stirring 20min is formed Colourless transparent solution；
(2) Ta of 47mg is weighed3N5Stirring is continued thereafter in the clear solution that nanoparticle is added in step (1) 10min, then by uniformly mixed suspension ultrasonic disperse 10min to get finely dispersed Ta3N5Nanoparticle mixed liquor；
(3) by finely dispersed Ta made from step (2)3N5Nano particle mixed liquor is transferred to the polytetrafluoroethylene (PTFE) of 100ml In reaction kettle, 8h is reacted at 160 DEG C, after reaction, is cooled to room temperature, the product secondary deionized water and nothing that will be obtained Water-ethanol washs for several times, and vacuum drying obtains CdIn2S4The Ta of the octahedra modification of nanometer3N5Nucleocapsid composite photo-catalyst, wherein CdIn2S4The octahedral mass fraction of nanometer is 50%.
(4) sample irradiates 210min under visible light, reaches 52.6% to the degradation efficiency of methyl orange.
Example 2:
(1) it is added according to 0.5:1:4 mMs than successively weighing four water cadmium nitrates, nitric hydrate indium and thioacetamide Into the ethanol water of 20mL, wherein the volume ratio of dehydrated alcohol and deionized water is 1:0.6, and stirring 20min forms colourless Clear solution；
(2) Ta of 156.7mg is weighed3N5Stirring is continued thereafter in the clear solution that nanoparticle is added in step (1) 15min, then by uniformly mixed suspension ultrasonic disperse 20min to get finely dispersed Ta3N5Nanoparticle mixed liquor；
(3) by finely dispersed Ta made from step (2)3N5Nano particle mixed liquor is transferred to the polytetrafluoroethylene (PTFE) of 100ml In reaction kettle, 12h is reacted at 170 DEG C, after reaction, is cooled to room temperature, by obtained product secondary deionized water and Dehydrated alcohol washs for several times, and vacuum drying obtains CdIn2S4The Ta of the octahedra modification of nanometer3N5Nucleocapsid composite photo-catalyst, Middle CdIn2S4The octahedral mass fraction of nanometer is 60%.
(4) sample irradiates 210min under visible light, reaches 68.3% to the degradation efficiency of methyl orange.
Scheme in attached drawing 1 of the invention according to the SEM of composite photocatalyst sample 2 made from example 2, can understand from figure Find out, CdIn2S4Nanometer octahedral structure, Ta is presented3N5For nanometer block structure, CdIn2S4Nanometer octahedron is by Ta3N5 Package is wherein, it was demonstrated that compound core-shell structure has become function preparation.
Example 3:
(1) it is added to according to 1:2:8 mMs than successively weighing four water cadmium nitrates, nitric hydrate indium and thioacetamide In the ethanol water of 30mL, wherein the volume ratio of dehydrated alcohol and deionized water is 1:0.7, and stirring 20min forms colourless Bright solution；
(2) Ta of 201.45mg is weighed3N5Stirring is continued thereafter in the clear solution that nanoparticle is added in step (1) 20min, then by uniformly mixed suspension ultrasonic disperse 25min to get finely dispersed Ta3N5Nanoparticle mixed liquor；
(3) by finely dispersed Ta made from step (2)3N5Nano particle mixed liquor is transferred to the polytetrafluoroethylene (PTFE) of 100ml In reaction kettle, 16h is reacted at 180 DEG C, after reaction, is cooled to room temperature, by obtained product secondary deionized water and Dehydrated alcohol washs for several times, and vacuum drying obtains CdIn2S4The Ta of the octahedra modification of nanometer3N5Nucleocapsid composite photo-catalyst, Middle CdIn2S4The octahedral mass fraction of nanometer is 70%.
(4) sample irradiates 210min under visible light, reaches 78.62% to the degradation efficiency of methyl orange.
Example 4:
(1) it is added according to 2:4:16 mMs than successively weighing four water cadmium nitrates, nitric hydrate indium and thioacetamide Into the ethanol water of 40mL, wherein the volume ratio of dehydrated alcohol and deionized water is 1:0.8, and stirring 20min forms colourless Clear solution；
(2) Ta of 235.2mg is weighed3N5Stirring is continued thereafter in the clear solution that nanoparticle is added in step (1) 25min, then by uniformly mixed suspension ultrasonic disperse 30min to get finely dispersed Ta3N5Nanoparticle mixed liquor；
(3) by finely dispersed Ta made from step (2)3N5Nano particle mixed liquor is transferred to the polytetrafluoroethylene (PTFE) of 100ml In reaction kettle, 22h is reacted at 190 DEG C, after reaction, is cooled to room temperature, by obtained product secondary deionized water and Dehydrated alcohol washs for several times, and vacuum drying obtains CdIn2S4The Ta of the octahedra modification of nanometer3N5Nucleocapsid composite photo-catalyst, Middle CdIn2S4The octahedral mass fraction of nanometer is 80%.
(4) sample irradiates 210min under visible light, reaches 92% to the degradation efficiency of methyl orange.
Scheme in attached drawing 4 of the invention according to the PL of composite photocatalyst sample 4 made from example 4, it can be clear from figure Find out, monomer CdIn2S4Nanometer octahedron shows very high PL intensity, it is meant that the compound speed of its internal electron carrier Rate is higher, introduces Ta3N5Later, greatly decaying occurs for the PL intensity of composite material, and it is compound that this result clearly shows this The building of structure greatly improves whole quantum efficiency, is beneficial to the significantly promotion of whole photocatalytic activity.
Example 5:
(1) it is added according to 3:6:24 mMs than successively weighing four water cadmium nitrates, nitric hydrate indium and thioacetamide Into the ethanol water of 50mL, wherein the volume ratio of dehydrated alcohol and deionized water is 1:0.9, and stirring 20min forms colourless Clear solution；
(2) Ta of 156.68mg is weighed3N5Stirring is continued thereafter in the clear solution that nanoparticle is added in step (1) 30min, then by uniformly mixed suspension ultrasonic disperse 35min to get finely dispersed Ta3N5Nanoparticle mixed liquor；
(3) by finely dispersed Ta made from step (2)3N5Nano particle mixed liquor is transferred to the polytetrafluoroethylene (PTFE) of 100ml In reaction kettle, 28h is reacted at 200 DEG C, after reaction, is cooled to room temperature, by obtained product secondary deionized water and Dehydrated alcohol washs for several times, and vacuum drying obtains CdIn2S4The Ta of the octahedra modification of nanometer3N5Nucleocapsid composite photo-catalyst, Middle CdIn2S4The octahedral mass fraction of nanometer is 90%.
(4) sample irradiates 210min under visible light, reaches 96.4% to the degradation efficiency of methyl orange.
According to the solid ultraviolet-ray visible absorbing light of composite photocatalyst sample 5 made from example 5 in attached drawing 3 of the invention Spectrogram, it can be seen from the figure that compared to monomer CdIn2S4For nano material, Ta is introduced3N5Later, the absorption of composite material Great red shift occurs for side, it was demonstrated that the composite catalyst is visible-light response type catalyst, possesses very strong visible light capture energy Power.
Example 6:
(1) it is added according to 4:8:32 mMs than successively weighing four water cadmium nitrates, nitric hydrate indium and thioacetamide Into the ethanol water of 60mL, wherein the volume ratio of dehydrated alcohol and deionized water is 1:1, and stirring 20min forms colourless Bright solution；
(2) Ta of 98.96mg is weighed3N5Stirring is continued thereafter in the clear solution that nanoparticle is added in step (1) 30min, then by uniformly mixed suspension ultrasonic disperse 40min to get finely dispersed Ta3N5Nanoparticle mixed liquor；
(3) by finely dispersed Ta made from step (2)3N5Nano particle mixed liquor is transferred to the polytetrafluoroethylene (PTFE) of 100ml In reaction kettle, 36h is reacted at 220 DEG C, after reaction, is cooled to room temperature, by obtained product secondary deionized water and Dehydrated alcohol washs for several times, and vacuum drying obtains CdIn2S4The Ta of the octahedra modification of nanometer3N5Nucleocapsid composite photo-catalyst, Middle CdIn2S4The octahedral mass fraction of nanometer is 89.3%.
(4) sample irradiates 210min under visible light, reaches 82.4% to the degradation efficiency of methyl orange.
Scheme in attached drawing 2 of the invention according to the TEM of composite photocatalyst sample 6 made from example 6, it can from figure Out, CdIn2S4Nanometer is octahedra to be closely attached to Ta3N5Core-shell structure is formed on nanometer blocks, further proves the composite material Successfully prepare.

Claims (7)

1.一种CdIn2S4纳米八面体修饰Ta3N5核壳复合光催化剂的制备方法，其特征在于，包括如下步骤：1. A preparation method of a CdIn 2 S 4 nano-octahedron modified Ta 3 N 5 core-shell composite photocatalyst, characterized in that, comprising the following steps: (1)按照一定的摩尔比依次称取四水硝酸镉、水合硝酸铟以及硫代乙酰胺加入到一定体积的乙醇水溶液中，搅拌形成无色透明溶液；(1) Weigh cadmium nitrate tetrahydrate, hydrated indium nitrate and thioacetamide sequentially according to a certain molar ratio, add them to a certain volume of ethanol aqueous solution, and stir to form a colorless transparent solution; (2)称取一定质量的Ta3N5纳米粒子加入到步骤(1)中的透明溶液中随后继续搅拌10-30min，再将混合均匀的悬浊液超声分散10-40min，即得分散均匀的Ta3N5纳米粒子混合液；(2) Weigh a certain mass of Ta 3 N 5 nanoparticles and add them to the transparent solution in step (1), then continue to stir for 10-30min, and then ultrasonically disperse the uniformly mixed suspension for 10-40min, to obtain uniform dispersion Ta 3 N 5 nanoparticle mixture; (3)将步骤(2)制得的分散均匀的Ta3N5纳米颗粒混合液转移至反应釜中反应一段时间，反应结束后，待冷却至室温，将得到的产物用二次去离子水和无水乙醇洗涤数次，真空干燥，得到CdIn2S4纳米八面体修饰的Ta3N5核壳复合光催化剂。(3) Transfer the uniformly dispersed Ta 3 N 5 nanoparticle mixed solution obtained in step (2) to the reaction kettle for a period of time, and after the reaction is completed, after cooling to room temperature, the obtained product is treated with secondary deionized water Washed with absolute ethanol for several times and dried in vacuum to obtain a Ta 3 N 5 core-shell composite photocatalyst modified by CdIn 2 S 4 nano-octahedron. 2.根据权利要求1所述的CdIn2S4纳米八面体修饰Ta3N5核壳复合光催化剂的制备方法，其特征在于，步骤(1)中，四水硝酸镉、水合硝酸铟以及硫代乙酰胺的毫摩尔比为(0.1-4):(0.2-8):(0.8-32)；其中四水硝酸镉与乙醇水溶液的用量比为0.1-4mmol:10-60mL。2. The preparation method of CdIn 2 S 4 nano-octahedral modified Ta 3 N 5 core-shell composite photocatalyst according to claim 1, wherein in step (1), cadmium nitrate tetrahydrate, hydrated indium nitrate and sulfur The millimolar ratio of acetamide is (0.1-4):(0.2-8):(0.8-32); wherein the consumption ratio of cadmium nitrate tetrahydrate and ethanol aqueous solution is 0.1-4mmol:10-60mL. 3.根据权利要求1所述的CdIn2S4纳米八面体修饰Ta3N5核壳复合光催化剂的制备方法，其特征在于，步骤(1)中，所述乙醇水溶液中，无水乙醇与去离子水的体积比为1:0.5-1；所述搅拌时间为20min。3. The preparation method of CdIn 2 S 4 nano-octahedron modified Ta 3 N 5 core-shell composite photocatalyst according to claim 1, wherein in step (1), in the ethanol aqueous solution, absolute ethanol and The volume ratio of deionized water is 1:0.5-1; the stirring time is 20min. 4.根据权利要求1所述的CdIn2S4纳米八面体修饰Ta3N5核壳复合光催化剂的制备方法，其特征在于，步骤(2)中，Ta3N5纳米粒子的粒径范围在300-600nm。4. The preparation method of CdIn 2 S 4 nano-octahedral modified Ta 3 N 5 core-shell composite photocatalyst according to claim 1, wherein in step (2), the particle size range of Ta 3 N 5 nanoparticles at 300-600nm. 5.根据权利要求1所述的CdIn2S4纳米八面体修饰Ta3N5核壳复合光催化剂的制备方法，其特征在于，步骤(3)中，反应温度控制在160-220℃，反应时间在8-36h。5 . The preparation method of CdIn 2 S 4 nano-octahedral modified Ta 3 N 5 core-shell composite photocatalyst according to claim 1 , wherein in step (3), the reaction temperature is controlled at 160-220° C., and the reaction The time is 8-36h. 6.根据权利要求1～5任一项所述制备方法制得的CdIn2S4纳米八面体修饰Ta3N5核壳复合光催化剂，其特征在于，所述复合光催化剂中CdIn2S4纳米八面体的质量分数在50-95％，CdIn2S4纳米八面体的边长在50-80nm。6 . The CdIn 2 S 4 nano-octahedral modified Ta 3 N 5 core-shell composite photocatalyst prepared according to the preparation method according to any one of claims 1 to 5, characterized in that, in the composite photocatalyst, CdIn 2 S 4 The mass fraction of nano-octahedron is 50-95%, and the side length of CdIn 2 S 4 nano-octahedron is 50-80 nm. 7.根据权利要求6所述的CdIn2S4纳米八面体修饰Ta3N5核壳复合光催化剂的应用，其特征在于，将所述的CdIn2S4纳米八面体修饰Ta3N5核壳复合光催化剂用于在可见光下催化氧化降解染料甲基橙。7. The application of the CdIn 2 S 4 nano-octahedron modified Ta 3 N 5 core-shell composite photocatalyst according to claim 6, wherein the Ta 3 N 5 core is modified by the CdIn 2 S 4 nano-octahedron The shell composite photocatalyst was used to catalyze the oxidative degradation of the dye methyl orange under visible light.
CN201811319448.4A 2018-11-07 2018-11-07 CdIn2S4 nano octahedron modified Ta3N5Preparation method of core-shell composite photocatalyst Active CN109499594B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811319448.4A CN109499594B (en) 2018-11-07 2018-11-07 CdIn2S4 nano octahedron modified Ta3N5Preparation method of core-shell composite photocatalyst

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811319448.4A CN109499594B (en) 2018-11-07 2018-11-07 CdIn2S4 nano octahedron modified Ta3N5Preparation method of core-shell composite photocatalyst

Publications (2)

Publication Number Publication Date
CN109499594A true CN109499594A (en) 2019-03-22
CN109499594B CN109499594B (en) 2021-11-23

Family

ID=65747781

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811319448.4A Active CN109499594B (en) 2018-11-07 2018-11-07 CdIn2S4 nano octahedron modified Ta3N5Preparation method of core-shell composite photocatalyst

Country Status (1)

Country Link
CN (1) CN109499594B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110124698A (en) * 2019-04-30 2019-08-16 江苏大学 A kind of CdIn2S4Nano-particle modified few layer MoS2The preparation method of nanometer sheet composite photo-catalyst
CN111203232A (en) * 2020-02-19 2020-05-29 江苏大学 SnIn4S8Preparation method of CdS protection type core-shell rod-shaped heterojunction composite photocatalyst

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003320366A (en) * 2002-05-02 2003-11-11 Nippon Steel Corp Method for cleaning contaminated soil
CN102423716A (en) * 2011-11-17 2012-04-25 北京科技大学 Preparation method and application of a heterojunction photocatalytic material uniformly coated with particles
CN103861630A (en) * 2014-03-12 2014-06-18 福州大学 Copolymerization-modified graphite-phase carbon nitride hollow ball visible light-driven photocatalyst
CN104826643A (en) * 2015-05-19 2015-08-12 浙江海洋学院 A Ta3N5/CdS heterojunction fiber photocatalyst and its preparation method
CN106622388A (en) * 2016-04-29 2017-05-10 杭州同净环境科技有限公司 Composite fiber material as well as preparation method and application thereof
CN107262115A (en) * 2017-06-29 2017-10-20 江苏大学 A kind of ZnO load Cs dIn2S4The preparation method and applications of the composite photo-catalyst of nano cubic block
CN108273539A (en) * 2018-02-07 2018-07-13 江苏大学 A kind of Ta3N5Nano particle hybridization TiO2Hollow ball composite photo-catalyst and its preparation method and application
CN108421551A (en) * 2018-02-07 2018-08-21 江苏大学 A kind of CdIn2S4Nano dot hydridization TiO2Hollow ball composite photo-catalyst and its preparation method and application
CN108525677A (en) * 2018-03-29 2018-09-14 中南民族大学 A kind of ceria/indium sulfide zinc nanometer sheet composite catalyst and its in visible light catalytic CO2Application in conversion

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003320366A (en) * 2002-05-02 2003-11-11 Nippon Steel Corp Method for cleaning contaminated soil
CN102423716A (en) * 2011-11-17 2012-04-25 北京科技大学 Preparation method and application of a heterojunction photocatalytic material uniformly coated with particles
CN103861630A (en) * 2014-03-12 2014-06-18 福州大学 Copolymerization-modified graphite-phase carbon nitride hollow ball visible light-driven photocatalyst
CN104826643A (en) * 2015-05-19 2015-08-12 浙江海洋学院 A Ta3N5/CdS heterojunction fiber photocatalyst and its preparation method
CN106622388A (en) * 2016-04-29 2017-05-10 杭州同净环境科技有限公司 Composite fiber material as well as preparation method and application thereof
CN107262115A (en) * 2017-06-29 2017-10-20 江苏大学 A kind of ZnO load Cs dIn2S4The preparation method and applications of the composite photo-catalyst of nano cubic block
CN108273539A (en) * 2018-02-07 2018-07-13 江苏大学 A kind of Ta3N5Nano particle hybridization TiO2Hollow ball composite photo-catalyst and its preparation method and application
CN108421551A (en) * 2018-02-07 2018-08-21 江苏大学 A kind of CdIn2S4Nano dot hydridization TiO2Hollow ball composite photo-catalyst and its preparation method and application
CN108525677A (en) * 2018-03-29 2018-09-14 中南民族大学 A kind of ceria/indium sulfide zinc nanometer sheet composite catalyst and its in visible light catalytic CO2Application in conversion

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110124698A (en) * 2019-04-30 2019-08-16 江苏大学 A kind of CdIn2S4Nano-particle modified few layer MoS2The preparation method of nanometer sheet composite photo-catalyst
CN110124698B (en) * 2019-04-30 2022-02-15 江苏大学 A preparation method of CdIn2S4 nanoparticle-modified few-layer MoS2 nanosheet composite photocatalyst
CN111203232A (en) * 2020-02-19 2020-05-29 江苏大学 SnIn4S8Preparation method of CdS protection type core-shell rod-shaped heterojunction composite photocatalyst

Also Published As

Publication number Publication date
CN109499594B (en) 2021-11-23

Similar Documents

Publication Publication Date Title
CN107456991B (en) A kind of preparation method of g-C3N4 quantum dot supported bismuth tungstate nanosheet photocatalyst
CN106902810A (en) Individual layer Bismuth tungstate nano-sheet composite photo-catalyst of carbon quantum dot modification and its preparation method and application
CN108993604B (en) AgIn5S8/UIO-66-NH2 composite material with high visible light activity and its preparation method and application
CN102698784B (en) Visible light response catalyst and preparation method thereof
CN106824070B (en) One kind two tungsten selenides-nitrogen-doped graphene photocatalysis adsorbent material and preparation method thereof
CN111250110A (en) Preparation method of visible light responsive SnIn4S8 nanoparticle/TiO2 nanobelt core-shell composite photocatalyst
CN113713831B (en) A copper-based heterojunction catalyst and its preparation method and application
CN106268881B (en) A kind of square block Ag2MoO4@Ag@AgBr ternary complex and its preparation method and application
CN107159264A (en) A kind of high-efficient full-spectrum response CuS/ graphene composite photocatalysts and preparation method thereof
CN108355669B (en) Magnetic nano onion carbon loaded Bi2WO6Photocatalyst and preparation method and application thereof
CN103191725A (en) BiVO4/Bi2WO6 compound semiconductor material and its hydrothermal preparation method and its application
Wu et al. Fabrication of Bi2MoO6/g-C3N4 visible-light driven photocatalyst for enhanced tetracycline degradation
CN110124690A (en) A kind of 1D Sb2S3Nanometer rods/3D ZnIn2S4The preparation method of composite construction
CN109663605A (en) A kind of binary 2D/2D CdIn2S4The preparation method and application of/BiOCl nano composite photo-catalyst
CN108421551A (en) A kind of CdIn2S4Nano dot hydridization TiO2Hollow ball composite photo-catalyst and its preparation method and application
CN106693996A (en) Preparation method and application for bismuth sulfide-bismuth ferrate composite visible-light photocatalyst
Shi et al. A magnetic recyclable MCM-48/ZnFe2O4/BiOBr heterojunction with improved RhB visible light degradation efficiency
CN114405522A (en) A ZnIn2S4/MoSe2 photocatalyst capable of efficiently reducing hexavalent chromium ions
CN105771962A (en) A near-infrared responsive carbon quantum dot/Bi2MoO6 photocatalyst and its preparation method
CN115845888B (en) Preparation method of PbBiO2Br/Ti3C2 composite catalyst and its application in photocatalytic degradation of methyl orange
Liu et al. Multi-mode photocatalytic performances of CdS QDs modified CdIn2S4/CdWO4 nanocomposites with high electron transfer ability
CN105056973A (en) Efficient Bi2S3-BiFeO3 composite visible-light-driven photocatalyst prepared through in-situ growth with chemical corrosion method and application of Bi2S3-BiFeO3 composite visible-light-driven photocatalyst
CN110404565A (en) A kind of titanium oxide/sulfur-rich vacancy molybdenum sulfide composite material and its preparation method and application
Li et al. Fabrication of Fe3O4@ Ti-PDA nanoparticles with enhanced photocatalytic activities for degradation of organic dye
CN109499594A (en) A kind of CdIn2S4 nanometers of octahedra modification Ta3N5The preparation method of nucleocapsid composite photo-catalyst

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right

Effective date of registration: 20240118

Address after: 712000 Factory Building 5, South Zone 1, Hongshengxing Aviation Technology Industrial Park, Dunhua Road, Airport New City, Xixian New Area, Xianyang City, Shaanxi Province

Patentee after: Xi'an Meinan Biotechnology Co.,Ltd.

Address before: 401329 No. 99, Xinfeng Avenue, Jinfeng Town, Gaoxin District, Jiulongpo District, Chongqing

Patentee before: Chongqing Science City Intellectual Property Operation Center Co.,Ltd.

Effective date of registration: 20240118

Address after: 401329 No. 99, Xinfeng Avenue, Jinfeng Town, Gaoxin District, Jiulongpo District, Chongqing

Patentee after: Chongqing Science City Intellectual Property Operation Center Co.,Ltd.

Address before: Zhenjiang City, Jiangsu Province, 212013 Jingkou District Road No. 301

Patentee before: JIANGSU University

TR01 Transfer of patent right