CN109521177A - A kind of preparation method of nano Au particle modification phosphorus sulphur codope grapheme material - Google Patents
A kind of preparation method of nano Au particle modification phosphorus sulphur codope grapheme material Download PDFInfo
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- CN109521177A CN109521177A CN201811113726.0A CN201811113726A CN109521177A CN 109521177 A CN109521177 A CN 109521177A CN 201811113726 A CN201811113726 A CN 201811113726A CN 109521177 A CN109521177 A CN 109521177A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Abstract
The invention discloses a kind of preparation methods of nano Au particle modification phosphorus sulphur codope grapheme material, its step includes the preparation of graphene oxide, phosphorus sulphur codope and nano Au particle modification, wherein the preparation of graphene oxide is divided into potassium chlorate oxidation stripping method or potassium permanganate oxidation stripping method, use phosphorus pentasulfide for phosphorus sulfur doping source, and using gold chloride as metal-modified agent.Nano Au particle made from this method, which modifies phosphorus sulphur codope grapheme material, has good heavy metal analysis ability, and detection sensitivity is high.
Description
Technical field
The present invention relates to technical field of graphene, especially a kind of nano Au particle modifies phosphorus sulphur codope grapheme material
Preparation method.
Background technique
Graphene is as a kind of novel two-dimension nano materials, since being found, it has been found that graphene is more next
More excellent properties, such as high strength & high electric-conduction, high sensing sensitivity etc..
Summary of the invention
The technical solution adopted by the present invention to solve the technical problems is: a kind of nano Au particle modification phosphorus sulphur codope stone
The preparation method of black alkene material, preparation, phosphorus sulphur codope and nano Au particle modification including graphene oxide, including walk as follows
It is rapid:
(1) 4g graphite powder is accurately weighed, is added to and fills beaker in 80~120ml sulfuric acid and 20~30ml nitric acid mixed liquor
In, the cooling 30~60min of ice-water bath in the case where constantly stirring；
(2) 15~69g of accumulated dose chloric acid is added every 5~10min in the beaker in the case where constantly stirring in step (1)
Beaker is sealed after potassium chlorate or potassium permanganate are added completely into, 4~8d is stirred at room temperature by potassium or potassium permanganate, obtains oxidation stone
Black alkene crude product；
(3) 1000ml deionized water is added in the graphene oxide crude product obtained to step (2), is heated to 60~80
DEG C, stir 30~60min；
(4) product that vacuum filtration step (3) obtains, and repeatedly eluted with hydrochloric acid solution, deionized water and dehydrated alcohol,
Until filtrate is clarified, pH value is neutral, obtains graphene oxide filter cake；
(5) the graphene oxide filter cake vacuum freeze-drying that will be obtained in step (4) obtains graphene oxide powder；
(6) the graphene oxide powder 100mg obtained in step (5) is accurately weighed, 100ml diethyl diethylene glycol dimethyl ether is added to
In, ultrasonic disperse handles 30~60min；
(7) addition 0.5~1.0ml pyridine in the decentralized system obtained to step (6), 1.0~3.0g phosphorus pentasulfide,
It is continually fed into ultrasonic disperse in the state that inert gas is protected and handles 30~60min；
(8) decentralized system that step (7) obtain is heated to 150~200 DEG C, keeps the temperature 30~120min, in heating process
It is continually fed into inert gas and is vigorously stirred, be cooled to room temperature after heat preservation；
(9) product that vacuum filtration (8) obtains, and eluted with acetone and deionized water, obtain filter cake；
(10) the filter cake vacuum freeze-drying for obtaining step (9) obtains phosphorus sulphur codope graphene；
(11) sodium citrate solution that 2ml mass fraction is 1% is accurately measured, the chlorine of 20ml concentration 1mmol/L is added drop-wise to
In auric acid solution, heating is boiled；
(12) the phosphorus sulphur codope graphene that 50~200mg of precise step (10) obtains, is added to step (11) and obtains
In the boiling solution obtained, ultrasonic disperse handles 30~60min, persistently stirs 6~12h afterwards, filters freeze-drying, acquisition nano Au particle
Modify phosphorus sulphur codope grapheme material.
A kind of preparation method of above-mentioned nano Au particle modification phosphorus sulphur codope grapheme material, the step graphite powder
Purity >=99.9%, the granularity of the graphite powder is 200~1000 mesh, the mass percent concentration of the sulfuric acid is 80~
90%, the mass percent concentration of the nitric acid is 60~70%, purity >=99.9% of the dehydrated alcohol, the acetone
Purity >=99.9%, purity >=99.9% of the step potassium permanganate, purity >=99.9% of the sodium citrate, the pyrrole
Purity >=99.9% of pyridine, purity >=99.99% of the gold chloride, purity >=99.9% of the potassium chlorate, the diethyl
Purity >=99.9% of diethylene glycol dimethyl ether, purity >=99.9% of the phosphorus pentasulfide, the mass percent of the hydrochloric acid solution
Concentration is 5~10%.
A kind of preparation method of above-mentioned nano Au particle modification phosphorus sulphur codope grapheme material, the inert gas are
The flow velocity that is passed through of argon gas or helium, the inert gas is 300~500mL/min.
A kind of preparation method of above-mentioned nano Au particle modification phosphorus sulphur codope grapheme material, the step ultrasound point
The frequency for dissipating processing is 20~40kHz, and power is 200~300W.
The invention has the advantages that the modification phosphorus sulphur codope grapheme material tool of nano Au particle made from this this method
There is good heavy metal analysis ability, detection sensitivity is high
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is the phosphorus sulphur codope graphene (HU-P) of embodiment 1 and the phosphorus sulphur codope graphite of embodiment 2 in the present invention
The Scanning Electron microscope photo of alkene (HO-P) compares；
Fig. 2 is the phosphorus sulphur codope graphene (HU-P) of embodiment 1 and the phosphorus sulphur codope graphite of embodiment 2 in the present invention
The elemental analysis photo comparison of alkene (HO-P)；
Fig. 3 is the phosphorus sulphur codope graphene (HU-P) of embodiment 1 and the phosphorus sulphur codope graphite of embodiment 2 in the present invention
The transmission electron microscope photo of alkene (HO-P) compares；
Fig. 4 be the present invention in embodiment 1 graphene oxide (HU-GO) and embodiment 2 graphene oxide (HO-GO),
The phosphorus sulphur codope graphene (HU-P) of embodiment 1 and the phosphorus sulphur codope graphene (HO-P) of embodiment 2, embodiment 1 are received
The nano Au particle of rice gold particle modification phosphorus sulphur codope graphene (HU-P-Au) and embodiment 2 modifies phosphorus sulphur codope graphite
The comparison of alkene (HO-P-Au) raman spectrum；
Fig. 5 is the phosphorus sulphur codope graphene (HU-P) of embodiment 1 and the phosphorus sulphur codope graphite of embodiment 2 in the present invention
The x-ray photoelectron spectroscopy spectrogram of alkene (HO-P) compares.
Specific embodiment
In order to illustrate more clearly of technical solution of the present invention, below the present invention is described further, it is clear that
Ground, disclosed below is only that section Example of the invention is not being paid for those of ordinary skill in the art
Under the premise of creative work, other embodiments are obtained according to these embodiments, belong to protection scope of the present invention.
[embodiment 1]
A kind of preparation method of nano Au particle modification phosphorus sulphur codope grapheme material, the system including graphene oxide
Standby, phosphorus sulphur codope and nano Au particle modification, include the following steps:
(1) 4g graphite powder is accurately weighed, is added to and fills in 115ml sulfuric acid and 30ml nitric acid mixed liquor in beaker, holding
The cooling 60min of lower ice-water bath is stirred continuously；
(2) accumulated dose 15g potassium permanganate is added every 10min in the beaker in the case where constantly stirring in step (1), to
Potassium permanganate seals beaker after being added completely into, and 5d is stirred at room temperature, and obtains graphene oxide crude product；
(3) 1000ml deionized water is added in the graphene oxide crude product obtained to step (2), is heated to 80 DEG C, stirs
Mix 60min；
(4) product that vacuum filtration step (3) obtains, and repeatedly eluted with hydrochloric acid solution, deionized water and dehydrated alcohol,
Until filtrate is clarified, pH value is neutral, obtains graphene oxide filter cake；
(5) the graphene oxide filter cake vacuum freeze-drying that will be obtained in step (4) obtains graphene oxide powder；
(6) the graphene oxide powder 100mg obtained in step (5) is accurately weighed, 100ml diethyl diethylene glycol dimethyl ether is added to
In, ultrasonic disperse handles 60min；
(7) 1.0ml pyridine is added in the decentralized system obtained to step (6), 3.0g phosphorus pentasulfide is lazy being continually fed into
Property gas protected in the state of ultrasonic disperse processing 60min；
(8) decentralized system that step (7) obtain is heated to 170 DEG C, keeps the temperature 60min, is continually fed into heating process lazy
Property gas is simultaneously vigorously stirred, and is cooled to room temperature after heat preservation；
(9) product that vacuum filtration (8) obtains, and eluted with acetone and deionized water, obtain filter cake；
(10) the filter cake vacuum freeze-drying for obtaining step (9) obtains phosphorus sulphur codope graphene；
(11) sodium citrate solution that 2ml mass fraction is 1% is accurately measured, the chlorine of 20ml concentration 1mmol/L is added drop-wise to
In auric acid solution, heating is boiled；
(12) the phosphorus sulphur codope graphene that precise 200mg step (10) obtains is added to step (11) acquisition
In boiling solution, ultrasonic disperse handles 60min, persistently stirs 12h afterwards, filters freeze-drying, and it is total to obtain nano Au particle modification phosphorus sulphur
Doped graphene material.
Detailed, purity >=99.9% of the step graphite powder, the granularity of the graphite powder is 1000 mesh, the sulfuric acid
Mass percent concentration be 80%, the mass percent concentration of the nitric acid is 68%, the purity of the dehydrated alcohol >=
99.9%, purity >=99.9% of the acetone, purity >=99.9% of the step potassium permanganate, the sodium citrate it is pure
Degree >=99.9%, purity >=99.9% of the pyridine, purity >=99.99% of the gold chloride, the purity of the potassium chlorate
>=99.9%, purity >=99.9% of the diethyl diethylene glycol dimethyl ether, purity >=99.9% of the phosphorus pentasulfide, the hydrochloric acid
The mass percent concentration of solution is 5%；The inert gas is argon gas, and the flow velocity that is passed through of the inert gas is 500mL/
min；The frequency of the step ultrasonic disperse processing is 40kHz, power 200W.
[embodiment 2]
A kind of preparation method of nano Au particle modification phosphorus sulphur codope grapheme material, the system including graphene oxide
Standby, phosphorus sulphur codope and nano Au particle modification, include the following steps:
(1) 4g graphite powder is accurately weighed, is added to and fills in 87.5ml sulfuric acid and 27ml nitric acid mixed liquor in beaker, holding
The cooling 30min of lower ice-water bath is stirred continuously；
(2) accumulated dose 55g potassium chlorate is added every 10min in the beaker in the case where constantly stirring in step (1), to chlorine
Sour potassium seals beaker after being added completely into, and 4d is stirred at room temperature, and obtains graphene oxide crude product；
(3) 1000ml deionized water is added in the graphene oxide crude product obtained to step (2), is heated to 70 DEG C, stirs
Mix 60min；
(4) product that vacuum filtration step (3) obtains, and repeatedly eluted with hydrochloric acid solution, deionized water and dehydrated alcohol,
Until filtrate is clarified, graphene oxide filter cake is obtained；
(5) the graphene oxide filter cake vacuum freeze-drying that will be obtained in step (4) obtains graphene oxide powder；
(6) the graphene oxide powder 100mg obtained in step (5) is accurately weighed, 100ml diethyl diethylene glycol dimethyl ether is added to
In, ultrasonic disperse handles 30min；
(7) 0.5ml pyridine is added in the decentralized system obtained to step (6), 1.0g phosphorus pentasulfide is lazy being continually fed into
Property gas protected in the state of ultrasonic disperse processing 30min；
(8) decentralized system that step (7) obtain is heated to 150 DEG C, keeps the temperature 30min, is continually fed into heating process lazy
Property gas is simultaneously vigorously stirred, and is cooled to room temperature after heat preservation；
(9) product that vacuum filtration (8) obtains, and eluted with acetone and deionized water, obtain filter cake；
(10) the filter cake vacuum freeze-drying for obtaining step (9) obtains phosphorus sulphur codope graphene；
(11) sodium citrate solution that 2ml mass fraction is 1% is accurately measured, the chlorine of 20ml concentration 1mmol/L is added drop-wise to
In auric acid solution, heating is boiled；
(12) the phosphorus sulphur codope graphene that precise 200mg step (10) obtains is added to step (11) acquisition
In boiling solution, ultrasonic disperse handles 30min, persistently stirs 6h afterwards, filters freeze-drying, obtains nano Au particle modification phosphorus sulphur and is co-doped with
Miscellaneous grapheme material.
Detailed, purity >=99.9% of the step graphite powder, the granularity of the graphite powder is 1000 mesh, the sulfuric acid
Mass percent concentration be 90%, the mass percent concentration of the nitric acid is 68%, the purity of the dehydrated alcohol >=
99.9%, purity >=99.9% of the acetone, purity >=99.9% of the step potassium permanganate, the sodium citrate it is pure
Degree >=99.9%, purity >=99.9% of the pyridine, purity >=99.99% of the gold chloride, the purity of the potassium chlorate
>=99.9%, purity >=99.9% of the diethyl diethylene glycol dimethyl ether, purity >=99.9% of the phosphorus pentasulfide, the hydrochloric acid
The mass percent concentration of solution is 5%；The inert gas be argon gas, the inert gas be passed through flow velocity be 300~
500mL/min；The frequency of the step ultrasonic disperse processing is 20kHz, power 300W.
Above embodiments are only exemplary embodiment of the present invention, are not used in the limitation present invention, protection scope of the present invention
It is defined by the claims.Those skilled in the art can within the spirit and scope of the present invention make respectively the present invention
Kind modification or equivalent replacement, this modification or equivalent replacement also should be regarded as being within the scope of the present invention.
Claims (4)
1. a kind of preparation method of nano Au particle modification phosphorus sulphur codope grapheme material, preparation including graphene oxide,
Phosphorus sulphur codope and nano Au particle modification, which comprises the steps of:
(1) 4g graphite powder is accurately weighed, is added to and fills in 80~120ml sulfuric acid and 20~30ml nitric acid mixed liquor in beaker,
Cooling 30~the 60min of ice-water bath in the case where constantly stirring；
(2) in the case where constantly stirring in beaker in step (1) every 5~10min be added 15~69g of accumulated dose potassium chlorate or
Beaker is sealed after potassium chlorate or potassium permanganate are added completely into, 4~8d is stirred at room temperature, obtains graphene oxide by potassium permanganate
Crude product；
(3) 1000ml deionized water is added in the graphene oxide crude product obtained to step (2), is heated to 60~80 DEG C, stirs
Mix 30~60min；
(4) product that vacuum filtration step (3) obtains, and repeatedly eluted with hydrochloric acid solution, deionized water and dehydrated alcohol, until
Filtrate clarification, pH value is neutral, obtains graphene oxide filter cake；
(5) the graphene oxide filter cake vacuum freeze-drying that will be obtained in step (4) obtains graphene oxide powder；
(6) the graphene oxide powder 100mg obtained in step (5) is accurately weighed, is added in 100ml diethyl diethylene glycol dimethyl ether,
Ultrasonic disperse handles 30~60min；
(7) 0.5~1.0ml pyridine is added in the decentralized system obtained to step (6), 1.0~3.0g phosphorus pentasulfide is continuing
It is passed through ultrasonic disperse in the state that inert gas is protected and handles 30~60min；
(8) decentralized system that step (7) obtain is heated to 150~200 DEG C, keeps the temperature 30~120min, continues in heating process
It is passed through inert gas and is vigorously stirred, be cooled to room temperature after heat preservation；
(9) product that vacuum filtration (8) obtains, and eluted with acetone and deionized water, obtain filter cake；
(10) the filter cake vacuum freeze-drying for obtaining step (9) obtains phosphorus sulphur codope graphene；
(11) sodium citrate solution that 2ml mass fraction is 1% is accurately measured, the gold chloride of 20ml concentration 1mmol/L is added drop-wise to
In solution, heating is boiled；
(12) the phosphorus sulphur codope graphene that 50~200mg of precise step (10) obtains is added to step (11) acquisition
In boiling solution, ultrasonic disperse handles 30~60min, persistently stirs 6~12h afterwards, filters freeze-drying, obtains nano Au particle modification
Phosphorus sulphur codope grapheme material.
2. a kind of preparation method of nano Au particle modification phosphorus sulphur codope grapheme material according to claim 1,
It is characterized in that, purity >=99.9% of the step graphite powder, the granularity of the graphite powder is 200~1000 mesh, the sulfuric acid
Mass percent concentration be 80~90%, the mass percent concentration of the nitric acid is 60~70%, the dehydrated alcohol
Purity >=99.9%, purity >=99.9% of the acetone, purity >=99.9% of the step potassium permanganate, the citric acid
Purity >=99.9% of sodium, purity >=99.9% of the pyridine, purity >=99.99% of the gold chloride, the potassium chlorate
Purity >=99.9%, purity >=99.9% of the diethyl diethylene glycol dimethyl ether, purity >=99.9% of the phosphorus pentasulfide, institute
The mass percent concentration for stating hydrochloric acid solution is 5~10%.
3. a kind of preparation method of nano Au particle modification phosphorus sulphur codope grapheme material according to claim 1,
It is characterized in that, the inert gas is argon gas or helium, and the flow velocity that is passed through of the inert gas is 300~500mL/min.
4. a kind of preparation method of nano Au particle modification phosphorus sulphur codope grapheme material according to claim 1,
It is characterized in that, the frequency of the step ultrasonic disperse processing is 20~40kHz, and power is 200~300W.
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Cited By (1)
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Application publication date: 20190326 |