CN106698526B - A kind of g-C3N4/FeS2The preparation method of nanocomposite - Google Patents
A kind of g-C3N4/FeS2The preparation method of nanocomposite Download PDFInfo
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- CN106698526B CN106698526B CN201710002931.9A CN201710002931A CN106698526B CN 106698526 B CN106698526 B CN 106698526B CN 201710002931 A CN201710002931 A CN 201710002931A CN 106698526 B CN106698526 B CN 106698526B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/12—Sulfides
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
The present invention provides a kind of g C3N4/FeS2The preparation method of nanocomposite, step are as follows：1st, g C are prepared3N4Powder；2nd, by g C3N4Powder is added in deionized water, ultrasonic disperse, obtains g C3N4Dispersion liquid；It weighs Iron dichloride tetrahydrate and is added to g C3N4In dispersion liquid, magnetic agitation dissolving obtains mixed liquor A；Under stiring, NaOH solution is added dropwise dropwise into mixed liquor A, obtains mixed liquid B；Thioacetyl amine aqueous solution is added dropwise into mixed liquid B, obtains mixed liquor C；Mixed liquor C is transferred in the stainless steel cauldron that polytetrafluoroethylene (PTFE) is liner, carries out solvent thermal reaction；After completion of the reaction, product is collected by centrifugation in cooled to room temperature, and product is washed with deionized water and absolute ethyl alcohol, dry, obtains g C3N4/FeS2Nanocomposite.Material prepared by method of the present invention can be applied to the fields such as lube oil additive, photoelectric material, hydrogen storage, photocatalysis.
Description
Technical field
Invention relates to field of nanocomposite materials, specifically, being a kind of g-C3N4/FeS2The preparation method of nanocomposite.
Background technology
In recent years, transition metal chalcogenide MX2(M=Mo, W, Nb etc.；X=S, Se, Te), due to its unique physics
Chemical property and novel structure, get more and more people's extensive concerning and further investigate, these substances 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 lubricating action, and iron is 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 with the deriving from a wealth of sources of polymer material, the relatively low advantage of price, but also 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, there is preferable photocatalysis performance, therefore is widely used as photochemical catalyst, such as
Photocatalysis degradation organic contaminant, photocatalysis liberation of hydrogen and photocatalysis organic synthesis etc..In addition, researcher employs pattern tune
The strategies such as control, element doping, semiconductors coupling effectively increase its photocatalytic activity.Recent studies have shown that g-C3N4It can increase
Original performance of strong composite material, therefore g-C3N4Based nano composite material lithium electricity, fuel sensitized cells, ultracapacitor and
The fields such as lubrication have potential application prospect.g-C3N4Although in intensity cannot be compared with graphene, it can be mild
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 height,
Unique electronic structure and class graphene film layer structure make its lubrication, catalyst carrier, sensor, organic reaction catalyst,
Photochemical catalyst, gas storage etc. 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/FeS2Nanocomposite can show its opposite homogenous material
More comprehensive, excellent performance.For nanocomposite, 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 nanocomposite,
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 nanocomposite, to improve curing
The performances such as electricity, calorifics, catalysis and the tribology of iron sum and extend its application field.
Technical solution is as follows：
A kind of g-C3N4/FeS2The preparation method of nanocomposite, step are as follows：
Step 1 prepares g-C3N4Powder；
Step 2 prepares g-C3N4/FeS2Nanocomposite：By g-C made from step 13N4Powder is added to deionized water
In, ultrasonic disperse obtains g-C3N4Dispersion liquid；It weighs Iron dichloride tetrahydrate and is added to g-C3N4In dispersion liquid, magnetic agitation is molten
Solution, obtains mixed liquor A；Under stiring, NaOH solution is added dropwise dropwise into mixed liquor A, obtains mixed liquid B；Into mixed liquid B
Thioacetyl amine aqueous solution is added dropwise, obtains mixed liquor C；Mixed liquor C is transferred to the stainless steel cauldron that polytetrafluoroethylene (PTFE) is liner
In, carry out solvent thermal reaction；After completion of the reaction, product is collected by centrifugation in cooled to room temperature, with deionized water and absolute ethyl alcohol
Product is washed, it is dry, obtain g-C3N4/FeS2Nanocomposite.
In step 1, g-C is prepared3N4The step of powder, is as follows：Urea is placed in corundum crucible with cover, is transferred to box electricity
It hinders in stove, is warming up to 550~600 DEG C, heating rate is 10 DEG C/min, keeps the temperature 2h, naturally cools to room temperature, obtain 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 volume ratio of used NaOH solution and mixed liquor A is 1:8, NaOH solution
Concentration is 0.75mol/L；In mixed liquor C, the mass ratio of the thioacetamide and the Iron dichloride tetrahydrate is 21:1, sulphur
Concentration for 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 for 24 hours.
In step 2, the rate of addition of the thioacetyl amine aqueous solution is 1 drop/sec.
Advantageous effect：
The advantages of synthetic method of the present invention is mild with reaction condition, simple for process, yield height and favorable reproducibility, it is made
Standby g-C3N4FeS2Nano-complex can be applied to the fields such as lube oil additive, photoelectric material, hydrogen storage, photocatalysis.
Description of the drawings
Fig. 1 is g-C prepared by embodiment 13N4With g-C3N4/FeS2The XRD diagram of nanocomposite.
Fig. 2 is g-C prepared by embodiment 13N4SEM figure.
Fig. 3 is g-C prepared by embodiment 13N4/FeS2Nanocomposite SEM schemes.
Fig. 4 is g-C prepared by embodiment 13N4/FeS2Nanocomposite TEM schemes.
Specific embodiment
Below in conjunction with the content that example further illustrates the present invention, 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：Using urea as raw material, 15g urea is placed in the corundum crucible with cover of 25mL, is transferred to
In chamber type electric resistance furnace, 550 DEG C are warming up to, heating rate is 10 DEG C/min, keeps the temperature 2h, naturally cools to room temperature, obtain faint yellow
g-C3N4Powder.
(2) g-C obtained in (1) is weighed3N4Powder 0.04g is added in 40mL deionized waters, is ultrasonically treated 30min, system
The dispersion liquid that concentration is 1.0mg/mL is obtained, is ultrasonically treated 30min.Then weigh four water 0.03g of frerrous chloride and be added to above-mentioned solution
In, magnetic agitation 5min, then, the NaOH solution 5ml that 0.75mol/L is measured with graduated cylinder are added drop-wise in above-mentioned dispersion liquid simultaneously dropwise
It is stirred continuously, weighs thioacetamide 0.63g and be placed in beaker after dissolving, obtain the solution of 0.40mol/L, be added drop-wise to dropwise
In above-mentioned mixed solution, finally mixed liquor is moved into the stainless steel cauldron that 100mL polytetrafluoroethylene (PTFE) is liner, in 200 DEG C
Under conditions of hydro-thermal for 24 hours, product is collected by centrifugation in cooled to room temperature, and product is washed with deionized water and absolute ethyl alcohol
It washs 6 times, finally the dry 12h at 60 DEG C, obtains black g-C3N4/FeS2Nano-complex.
G-C in Fig. 13N4With g-C3N4/FeS2Characteristic peak have and coincide well, and without the appearance of other miscellaneous peaks,
Illustrate g-C compound in step 23N4/FeS2Nano-complex has very high purity.Fig. 2 indicates the g-C synthesized in step 13N4For
Nano-sheet substance.Fig. 3,4 show ferrous disulfide and have been compounded in g-C well3N4Surface.
Embodiment 2：
(1)g-C3N4Preparation：Using urea as raw material, 15g urea is placed in the corundum crucible with cover of 25mL, is transferred to
In chamber type electric resistance furnace, 550 DEG C are warming up to, heating rate is 20 DEG C/min, keeps the temperature 2h, naturally cools to room temperature, obtain faint yellow
g-C3N4Powder.
(2) g-C obtained in (1) is weighed3N4Powder 0.02g is added in 40mL deionized waters, is ultrasonically treated 30min, system
The dispersion liquid that concentration is 1.0mg/mL is obtained, is ultrasonically treated 30min.Then weigh four water 0.03g of frerrous chloride and be added to above-mentioned solution
In, magnetic agitation 5min, then, the NaOH solution 5ml that 0.75mol/L is measured with graduated cylinder are added drop-wise in above-mentioned dispersion liquid simultaneously dropwise
It is stirred continuously, weighs thioacetamide 0.63g and be placed in beaker after dissolving, obtain the solution of 0.40mol/L, be added drop-wise to dropwise
In above-mentioned mixed solution, finally mixed liquor is moved into the stainless steel cauldron that 100mL polytetrafluoroethylene (PTFE) is liner, in 200 DEG C
Under conditions of hydro-thermal for 24 hours, product is collected by centrifugation in cooled to room temperature, and product is washed with deionized water and absolute ethyl alcohol
It washs 6 times, finally the dry 12h at 60 DEG C, obtains black g-C3N4/FeS2Nano-complex.
Embodiment 3：
(1)g-C3N4Preparation：Using urea as raw material, 15g urea is placed in the corundum crucible with cover of 25mL, is transferred to
In chamber type electric resistance furnace, 550 DEG C are warming up to, heating rate is 10 DEG C/min, keeps the temperature 2h, naturally cools to room temperature, obtain faint yellow
g-C3N4Powder.
(2) g-C obtained in (1) is weighed3N4Powder 0.08g is added in 40mL deionized waters, is ultrasonically treated 30min, system
The dispersion liquid that concentration is 1.0mg/mL is obtained, is ultrasonically treated 30min.Then weigh four water 0.03g of frerrous chloride and be added to above-mentioned solution
In, magnetic agitation 5min, then, the NaOH solution 5ml that 0.75mol/L is measured with graduated cylinder are added drop-wise in above-mentioned dispersion liquid simultaneously dropwise
It is stirred continuously, weighs thioacetamide 0.63g and be placed in beaker after dissolving, obtain the solution of 0.40mol/L, be added drop-wise to dropwise
In above-mentioned mixed solution, finally mixed liquor is moved into the stainless steel cauldron that 100mL polytetrafluoroethylene (PTFE) is liner, in 200 DEG C
Under conditions of hydro-thermal for 24 hours, product is collected by centrifugation in cooled to room temperature, and product is washed with deionized water and absolute ethyl alcohol
It washs 6 times, finally the dry 12h at 60 DEG C, obtains black g-C3N4/FeS2Nano-complex.
Claims (5)
1. a kind of g-C3N4/FeS2The preparation method of nanocomposite, which is characterized in that step is as follows：
Step 1 prepares g-C3N4Powder；
Step 2 prepares g-C3N4/FeS2Nanocomposite：By g-C made from step 13N4Powder is added in deionized water,
Ultrasonic disperse obtains g-C3N4Dispersion liquid；It weighs Iron dichloride tetrahydrate and is added to g-C3N4In dispersion liquid, magnetic agitation dissolving,
Obtain mixed liquor A；Under stiring, NaOH solution is added dropwise dropwise into mixed liquor A, obtains mixed liquid B；It is added dropwise into 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, into
Row solvent thermal reaction；After completion of the reaction, product is collected by centrifugation in cooled to room temperature, with deionized water and absolute ethyl alcohol to production
Object is washed, dry, obtains g-C3N4/FeS2Nanocomposite；
In mixed liquid B, the volume ratio of used NaOH solution and mixed liquor A is 1:8, the concentration of NaOH solution is 0.75mol/
L。
2. a kind of g-C according to claim 13N4/FeS2The preparation method of nanocomposite, which is characterized 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, is heated up
To 550 ~ 600 DEG C, heating rate is 10 DEG C/min, keeps the temperature 2h, naturally cools to room temperature, obtain faint yellow g-C3N4Powder.
3. a kind of g-C according to claim 13N4/FeS2The preparation method of nanocomposite, which is characterized 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 liquor C, the mass ratio of the thioacetamide and the Iron dichloride tetrahydrate is 21:1, thioacetyl amine aqueous solution
Concentration be 0.40mol/L.
4. a kind of g-C according to claim 13N4/FeS2The preparation method of nanocomposite, which is characterized in that step
In 2, the temperature of the solvent thermal reaction is 200 DEG C, and the reaction time is for 24 hours.
5. a kind of g-C according to claim 13N4/FeS2The preparation method of nanocomposite, which is characterized in that step
In 2, the rate of addition of the thioacetyl amine aqueous solution is 1 drop/sec.
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| CN110918102A (en) * | 2019-12-10 | 2020-03-27 | 桂林理工大学 | Preparation method of graphene oxide modified metal sulfide composite photocatalyst |
| CN111111734B (en) * | 2019-12-30 | 2022-08-09 | 江南大学 | Preparation and application of ferrous disulfide/carbon nitride composite photocatalyst |
| 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 |
| 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 |
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