CN106698526A - Method for preparing g-C3N4/FeS2 nano composite material - Google Patents
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention provides a method for preparing a g-C3N4/FeS2 nano composite material. The method comprises the following steps: 1, preparing g-C3N4 powder; 2, adding the g-C3N4 powder into deionized water, and performing ultrasonic dispersion so as to obtain a g-C3N4 dispersion liquid; weighing iron dichloride tetrahydrate, adding into the g-C3N4 dispersion liquid, performing magnetic stirring dissolution so as to obtain a mixed liquid A; dropping a NaOH solution into the mixed liquid A one by one with stirring so as to obtain a mixed liquid B; dropping a thioacetamide solution into the mixed liquid B one by one so as to obtain a mixed liquid C; transferring the mixed liquid C into a stainless steel reaction kettle with polytetrafluoroethylene as a liner, and performing a solvent thermal reaction; and after the reaction is completed, naturally cooling to the room temperature, centrifuging and collecting a product, washing a product by using deionized water and absolute ethyl alcohol, and drying, thereby obtaining the g-C3N4/FeS2 nano composite material. The material prepared by using the method provided by the invention can be applied to fields such as lubricant additives, photoelectric materials, hydrogen storage, photocatalysis and the like.
Description
Technical field
Invention relates to field of nanocomposite materials, specifically, being a kind of g-C3N4/FeS2The preparation method of nano composite material.
Background technology
In recent years, transition metal chalcogenide MX2(M=Mo, W, Nb etc.；X=S, Se, Te), due to its unique physics
The structure of chemical property and novelty, gets more and more people's extensive concerning and furthers investigate, and these materials are widely used as lithium-ion electric
Pond electrode, lube oil additive, new catalyst and thermoelectric material etc., wherein, FeS2As in transition metal chalcogenide
Important a member, many peculiar properties are made it have due to its special crystal structure, especially as magnesium-yttrium-transition metal sulphur
Compound nano particle makes it possess certain anti-attrition lubrication, and iron as its curing of the element of rich reserves on the earth
There are very big potentiality in the commercial Application of iron.
g-C3N4It is a kind of polymer semiconductor similar to graphene-structured, C, N atom are with sp2Hydridization formed height from
The pi-conjugated system in domain.g-C3N4Not only there is wide material sources, the relatively low advantage of price of polymeric material, and its excellent light is urged
Changing performance can also compare favourably with traditional inorganic semiconductor catalysis material.g-C3N4Because of its unique band structure and excellent change
Stability is learned, and has certain absorption to visible ray, with preferable photocatalysis performance, therefore be widely used as photochemical catalyst, such as
Photocatalysis degradation organic contaminant, photocatalysis liberation of hydrogen and photocatalysis organic synthesis etc..Additionally, researcher employs pattern tune
The strategies such as control, element doping, semiconductors coupling, effectively increase its photocatalytic activity.Recent studies have shown that, g-C3N4Can increase
Original performance of strong composite, therefore g-C3N4Based nano composite material lithium electricity, fuel sensitized cells, ultracapacitor and
The fields such as lubrication have potential application prospect.g-C3N4Although can not be compared with Graphene in intensity, it can be gentle
Under conditions of carried out by a series of predecessor (melamine etc.) of carbon containing rich nitrogen it is a large amount of synthetically prepared, the stability of its height,
Unique electronic structure and class graphene film Rotating fields make its lubrication, catalyst carrier, sensor, organic reaction catalyst,
The aspects such as photochemical catalyst, gas storage have very huge potential using value, and are seen as most being hopeful to supplement carbon materials
Expect the material in many aspect potential applications, thus cause domestic and foreign scholars and researcher to this with unlimited potentiality
The tireless exploration of new material.
Based on g-C3N4、FeS2Good characteristic, g-C3N4/FeS2Nano composite material can show relative its homogenous material
More comprehensive, excellent performance.For nano composite material, research concentrates on graphene-based nano combined material mostly at present
Material, such as Graphene/ferrous disulfide nanocomposite material, and in g-C3N4The research in based nano composite material field is less, and focuses mostly on
In g-C3N4Light-catalysed application.Therefore, the invention discloses a kind of g-C3N4/FeS2The preparation method of nano composite material,
And there is good development prospect in fields such as tribology, catalysis, lithium electricity.
The content of the invention
It is an object of the invention to provide a kind of g-C3N4/FeS2The preparation method of nano composite material, to improve curing
The performances such as the electricity of iron sum, calorifics, catalysis and tribology and extend its application field.
Technical scheme is as follows：
A kind of g-C3N4/FeS2The preparation method of nano composite material, step is as follows：
Step 1, preparation g-C3N4Powder；
Step 2, preparation g-C3N4/FeS2Nano composite material：By g-C obtained in step 13N4Powder is added to deionized water
In, ultrasonic disperse obtains g-C3N4Dispersion liquid；Weigh Iron dichloride tetrahydrate and be added to g-C3N4In dispersion liquid, magnetic agitation is molten
Solution, obtains mixed liquor A；Under agitation, to NaOH solution is dropwise added dropwise in mixed liquor A, mixed liquid B is obtained；Dripped in mixed liquid B
Plus thioacetyl amine aqueous solution, obtain mixed liquor C；Mixed liquor C is transferred in the stainless steel cauldron that polytetrafluoroethylene (PTFE) is liner,
Carry out solvent thermal reaction；After completion of the reaction, room temperature is naturally cooled to, product is collected by centrifugation, with deionized water and absolute ethyl alcohol pair
Product is washed, and is dried, and obtains g-C3N4/FeS2Nano composite material.
In step 1, g-C is prepared3N4The step of powder, is as follows：Urea is placed in corundum crucible with cover, box electricity is transferred to
In resistance stove, 550~600 DEG C are warming up to, heating rate is 10 DEG C/min, is incubated 2h, naturally cools to room temperature, obtains faint yellow g-
C3N4Powder.
In step 2, g-C3N4The concentration of dispersion liquid is 0.5~2mg/mL；In mixed liquor A, the Iron dichloride tetrahydrate
Concentration is 0.75mg/mL；In mixed liquid B, the NaOH solution for being used is 1 with the volume ratio of mixed liquor A:8, NaOH solution it is dense
It is 0.75mol/L to spend；In mixed liquor C, the thioacetamide is 21 with the mass ratio of the Iron dichloride tetrahydrate:1, it is thio
The concentration of acetamide solution is 0.40mol/L.
In step 2, the temperature of the solvent thermal reaction is 200 DEG C, and the reaction time is 24h.
In step 2, the rate of addition of the thioacetyl amine aqueous solution is 1 drop/sec.
Beneficial effect：
Synthetic method of the invention has reaction condition gentle, process is simple, and yield is high and advantage of favorable reproducibility, made
Standby g-C3N4FeS2Nano-complex can be applied to the fields such as lube oil additive, photoelectric material, hydrogen storage, photocatalysis.
Brief description of the drawings
Fig. 1 is g-C prepared by embodiment 13N4With g-C3N4/FeS2The XRD of nano composite material.
Fig. 2 is g-C prepared by embodiment 13N4SEM figure.
Fig. 3 is g-C prepared by embodiment 13N4/FeS2Nano composite material SEM schemes.
Fig. 4 is g-C prepared by embodiment 13N4/FeS2Nano composite material TEM schemes.
Specific embodiment
Present disclosure is further illustrated below in conjunction with example, as known by the technical knowledge, the present invention also can be by other
The scheme that does not depart from the technology of the present invention feature describe, it is therefore all within the scope of the present invention or in the equivalent scope of the invention
Change is included in the invention.
Embodiment 1：
(1)g-C3N4Preparation：With urea as raw material, 15g urea is placed in the corundum crucible with cover of 25mL, be transferred to
In chamber type electric resistance furnace, 550 DEG C are warming up to, programming rate is 10 DEG C/min, is incubated 2h, naturally cools to room temperature, obtains faint yellow
g-C3N4Powder.
(2) obtained g-C in (1) is weighed3N4Powder 0.04g is added in 40mL deionized waters, ultrasonically treated 30min, system
It is the dispersion liquid of 1.0mg/mL, ultrasonically treated 30min to obtain concentration.Then weigh the water 0.03g of frerrous chloride four and be added to above-mentioned solution
In, magnetic agitation 5min, then, the NaOH solution 5ml for measuring 0.75mol/L with graduated cylinder is dropwise added drop-wise in above-mentioned dispersion liquid simultaneously
It is stirred continuously, weighs thioacetamide 0.63g and be placed in beaker after dissolving, obtain the solution of 0.40mol/L, is dropwise added drop-wise to
In above-mentioned mixed solution, during mixed liquor finally is moved into 100mL polytetrafluoroethylene (PTFE) for the stainless steel cauldron of liner, in 200 DEG C
Under conditions of hydro-thermal 24h, naturally cool to room temperature, product is collected by centrifugation, product is washed with deionized water and absolute ethyl alcohol
Wash 6 times, finally dry 12h at 60 DEG C, obtain black g-C3N4/FeS2Nano-complex.
G-C in Fig. 13N4With g-C3N4/FeS2Characteristic peak have and coincide well, and the appearance without other miscellaneous peaks,
Illustrate the g-C being combined in step 23N4/FeS2Nano-complex has purity very high.Fig. 2 indicates the g-C synthesized in step 13N4For
Nano-sheet material.Fig. 3,4 indicate ferrous disulfide and have been compounded in g-C well3N4Surface.
Embodiment 2：
(1)g-C3N4Preparation：With urea as raw material, 15g urea is placed in the corundum crucible with cover of 25mL, be transferred to
In chamber type electric resistance furnace, 550 DEG C are warming up to, programming rate is 20 DEG C/min, is incubated 2h, naturally cools to room temperature, obtains faint yellow
g-C3N4Powder.
(2) obtained g-C in (1) is weighed3N4Powder 0.02g is added in 40mL deionized waters, ultrasonically treated 30min, system
It is the dispersion liquid of 1.0mg/mL, ultrasonically treated 30min to obtain concentration.Then weigh the water 0.03g of frerrous chloride four and be added to above-mentioned solution
In, magnetic agitation 5min, then, the NaOH solution 5ml for measuring 0.75mol/L with graduated cylinder is dropwise added drop-wise in above-mentioned dispersion liquid simultaneously
It is stirred continuously, weighs thioacetamide 0.63g and be placed in beaker after dissolving, obtain the solution of 0.40mol/L, is dropwise added drop-wise to
In above-mentioned mixed solution, during mixed liquor finally is moved into 100mL polytetrafluoroethylene (PTFE) for the stainless steel cauldron of liner, in 200 DEG C
Under conditions of hydro-thermal 24h, naturally cool to room temperature, product is collected by centrifugation, product is washed with deionized water and absolute ethyl alcohol
Wash 6 times, finally dry 12h at 60 DEG C, obtain black g-C3N4/FeS2Nano-complex.
Embodiment 3：
(1)g-C3N4Preparation：With urea as raw material, 15g urea is placed in the corundum crucible with cover of 25mL, be transferred to
In chamber type electric resistance furnace, 550 DEG C are warming up to, programming rate is 10 DEG C/min, is incubated 2h, naturally cools to room temperature, obtains faint yellow
g-C3N4Powder.
(2) obtained g-C in (1) is weighed3N4Powder 0.08g is added in 40mL deionized waters, ultrasonically treated 30min, system
It is the dispersion liquid of 1.0mg/mL, ultrasonically treated 30min to obtain concentration.Then weigh the water 0.03g of frerrous chloride four and be added to above-mentioned solution
In, magnetic agitation 5min, then, the NaOH solution 5ml for measuring 0.75mol/L with graduated cylinder is dropwise added drop-wise in above-mentioned dispersion liquid simultaneously
It is stirred continuously, weighs thioacetamide 0.63g and be placed in beaker after dissolving, obtain the solution of 0.40mol/L, is dropwise added drop-wise to
In above-mentioned mixed solution, during mixed liquor finally is moved into 100mL polytetrafluoroethylene (PTFE) for the stainless steel cauldron of liner, in 200 DEG C
Under conditions of hydro-thermal 24h, naturally cool to room temperature, product is collected by centrifugation, product is washed with deionized water and absolute ethyl alcohol
Wash 6 times, finally dry 12h at 60 DEG C, obtain black g-C3N4/FeS2Nano-complex.
Claims (5)
1. a kind of g-C3N4/FeS2The preparation method of nano composite material, it is characterised in that step is as follows：
Step 1, preparation g-C3N4Powder；
Step 2, preparation g-C3N4/FeS2Nano composite material：By g-C obtained in step 13N4Powder is added in deionized water,
Ultrasonic disperse, obtains g-C3N4Dispersion liquid；Weigh Iron dichloride tetrahydrate and be added to g-C3N4In dispersion liquid, magnetic agitation dissolving,
Obtain mixed liquor A；Under agitation, to NaOH solution is dropwise added dropwise in mixed liquor A, mixed liquid B is obtained；It is added dropwise in mixed liquid B
Thioacetyl amine aqueous solution, obtains mixed liquor C；Mixed liquor C is transferred in the stainless steel cauldron that polytetrafluoroethylene (PTFE) is liner, is entered
Row solvent thermal reaction；After completion of the reaction, room temperature is naturally cooled to, product is collected by centrifugation, with deionized water and absolute ethyl alcohol to producing
Thing is washed, and is dried, and obtains g-C3N4/FeS2Nano composite material.
2. a kind of g-C according to claim 13N4/FeS2The preparation method of nano composite material, it is characterised in that step
In 1, g-C is prepared3N4The step of powder, is as follows：Urea is placed in corundum crucible with cover, is transferred in chamber type electric resistance furnace, heated up
To 550~600 DEG C, heating rate is 10 DEG C/min, is incubated 2h, naturally cools to room temperature, obtains faint yellow g-C3N4Powder.
3. a kind of g-C according to claim 13N4/FeS2The preparation method of nano composite material, it is characterised in that step
In 2, g-C3N4The concentration of dispersion liquid is 0.5~2mg/mL；In mixed liquor A, the concentration of the Iron dichloride tetrahydrate is
0.75mg/mL；In mixed liquid B, the NaOH solution for being used is 1 with the volume ratio of mixed liquor A:8, the concentration of NaOH solution is
0.75mol/L；In mixed liquor C, the thioacetamide is 21 with the mass ratio of the Iron dichloride tetrahydrate:1, thioacetyl
The concentration of amine aqueous solution is 0.40mol/L.
4. a kind of g-C according to claim 13N4/FeS2The preparation method of nano composite material, it is characterised in that step
In 2, the temperature of the solvent thermal reaction is 200 DEG C, and the reaction time is 24h.
5. a kind of g-C according to claim 13N4/FeS2The preparation method of nano composite material, it is characterised in that step
In 2, the rate of addition of the thioacetyl amine aqueous solution is 1 drop/sec.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110075896A (en) * | 2019-04-09 | 2019-08-02 | 重庆大学 | FeS2/g-C3N4The preparation method and applications of heterojunction material |
| CN110918102A (en) * | 2019-12-10 | 2020-03-27 | 桂林理工大学 | Preparation method of graphene oxide modified metal sulfide composite photocatalyst |
| CN111111734A (en) * | 2019-12-30 | 2020-05-08 | 江南大学 | Preparation and application of ferrous disulfide/carbon nitride composite photocatalyst |
| CN113083006A (en) * | 2021-03-26 | 2021-07-09 | 上海师范大学 | C for degrading NO by gas-solid phase photoelectric Fenton3N4Fe(1-x)Preparation method and application of S stainless steel electrode composite material |
| CN113611835A (en) * | 2021-07-31 | 2021-11-05 | 青岛科技大学 | g-C3N4@WS2Electroactive material, method for the production thereof and use thereof |
| CN113896817A (en) * | 2021-10-26 | 2022-01-07 | 茂名实华东成化工有限公司 | g-C3N4/MgCl2Preparation method of composite carrier type propylene polymerization catalyst |
| CN115318327A (en) * | 2022-08-17 | 2022-11-11 | 中化学朗正环保科技有限公司 | Preparation method of heterogeneous catalyst for treating near-neutral organic wastewater |
| CN115888791A (en) * | 2022-11-14 | 2023-04-04 | 武汉轻工大学 | High-stability pyrrhotite photo-Fenton catalyst, and preparation method and application thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110075896A (en) * | 2019-04-09 | 2019-08-02 | 重庆大学 | FeS2/g-C3N4The preparation method and applications of heterojunction material |
| CN110075896B (en) * | 2019-04-09 | 2021-12-07 | 重庆大学 | FeS2/g-C3N4Preparation method and application of heterojunction material |
| CN110918102A (en) * | 2019-12-10 | 2020-03-27 | 桂林理工大学 | Preparation method of graphene oxide modified metal sulfide composite photocatalyst |
| CN111111734A (en) * | 2019-12-30 | 2020-05-08 | 江南大学 | Preparation and application of ferrous disulfide/carbon nitride composite photocatalyst |
| CN111111734B (en) * | 2019-12-30 | 2022-08-09 | 江南大学 | Preparation and application of ferrous disulfide/carbon nitride composite photocatalyst |
| CN113083006A (en) * | 2021-03-26 | 2021-07-09 | 上海师范大学 | C for degrading NO by gas-solid phase photoelectric Fenton3N4Fe(1-x)Preparation method and application of S stainless steel electrode composite material |
| CN113083006B (en) * | 2021-03-26 | 2023-01-17 | 上海师范大学 | C for degrading NO by gas-solid phase photoelectric Fenton 3 N 4 Fe (1-x) Preparation method and application of S stainless steel electrode composite material |
| CN113611835A (en) * | 2021-07-31 | 2021-11-05 | 青岛科技大学 | g-C3N4@WS2Electroactive material, method for the production thereof and use thereof |
| CN113896817A (en) * | 2021-10-26 | 2022-01-07 | 茂名实华东成化工有限公司 | g-C3N4/MgCl2Preparation method of composite carrier type propylene polymerization catalyst |
| CN113896817B (en) * | 2021-10-26 | 2022-12-02 | 茂名实华东成化工有限公司 | g-C 3 N 4 /MgCl 2 Preparation method of composite carrier type propylene polymerization catalyst |
| CN115318327A (en) * | 2022-08-17 | 2022-11-11 | 中化学朗正环保科技有限公司 | Preparation method of heterogeneous catalyst for treating near-neutral organic wastewater |
| CN115888791A (en) * | 2022-11-14 | 2023-04-04 | 武汉轻工大学 | High-stability pyrrhotite photo-Fenton catalyst, and preparation method and application thereof |
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