CN109607500A - A kind of g-C3N4The preparation method of ultrathin nanometer piece - Google Patents
A kind of g-C3N4The preparation method of ultrathin nanometer piece Download PDFInfo
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- CN109607500A CN109607500A CN201811640311.9A CN201811640311A CN109607500A CN 109607500 A CN109607500 A CN 109607500A CN 201811640311 A CN201811640311 A CN 201811640311A CN 109607500 A CN109607500 A CN 109607500A
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- centrifugal treating
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- melamine
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- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 52
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000001035 drying Methods 0.000 claims abstract description 38
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000007864 aqueous solution Substances 0.000 claims abstract description 25
- 238000000137 annealing Methods 0.000 claims abstract description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 59
- 239000008367 deionised water Substances 0.000 claims description 29
- 229910021641 deionized water Inorganic materials 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 24
- 239000007787 solid Substances 0.000 claims description 22
- 239000000376 reactant Substances 0.000 claims description 18
- 238000004140 cleaning Methods 0.000 claims description 16
- 239000007795 chemical reaction product Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000010410 layer Substances 0.000 abstract description 26
- 239000003054 catalyst Substances 0.000 abstract description 7
- 239000002086 nanomaterial Substances 0.000 abstract description 6
- 239000007789 gas Substances 0.000 abstract description 4
- 239000002060 nanoflake Substances 0.000 abstract description 3
- 239000002365 multiple layer Substances 0.000 abstract description 2
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 239000013618 particulate matter Substances 0.000 abstract 1
- 238000001816 cooling Methods 0.000 description 20
- 239000000463 material Substances 0.000 description 19
- 238000005119 centrifugation Methods 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- 239000004570 mortar (masonry) Substances 0.000 description 10
- 239000010453 quartz Substances 0.000 description 10
- 230000004044 response Effects 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 238000000034 method Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000002305 electric material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0259—Compounds of N, P, As, Sb, Bi
-
- 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
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention discloses a kind of g-C3N4The preparation method of ultrathin nanometer piece: after product cleaning-centrifugal treating after melamine aqueous solution to be carried out to hydro-thermal reaction, low temperature drying, grinding obtains g-C3N4Predecessor particulate matter is made annealing treatment under nitrogen protection atmosphere, obtains g-C3N4Ultrathin nanometer piece；G-C prepared by the present invention3N4Ultrathin nanometer chip architecture has unique shape characteristic, two-dimensional ultrathin nanostructure made of being stacked for a large amount of few layer (3-5 layers) sheet, its pattern is uniform and surface is smooth, can provide more activated adoption sites, be conducive to the quick adsorption of organic pollutant molecule；Secondly, a large amount of nano flake stacks the structure to be formed and greatly increases its specific surface area, and multiple-layer stacked structure can enhance its mechanical strength, the stability of its long-time service certainly will be improved, which all has good application prospect in terms of gas sensing, photochemical catalyst and catalyst carrier.
Description
Technical field
The present invention relates to nanotechnology, materials chemistry and environmental science cross-application fields, and in particular to a kind of g-C3N4It is super
The preparation method of thin nanometer chip architecture.
Background technique
In recent years, since problem of environmental pollution increasingly sharpens, contaminant gases are quickly detected or difficult decomposing organic matter is quick
The research of degradation aspect becomes the hot spot paid close attention to both at home and abroad.In addition, due to a variety of drugs, chemical products in modern industrial process
Abuse and the burning of byproduct cause a large amount of pollutants to accumulate and discharge wantonly in the environment, pollutant chemistry property is steady
It is fixed, in the environment can long-term existence, seriously threatened the health of the mankind.
Two-dimensional semiconductor nano material is due to biggish specific surface area and unique space structure and adjustable light
Catalytic property, chemical property, efficient degradation rate and it is environmental-friendly the features such as, be always air-sensitive catalyst, photochemical catalyst
Candidate material.In addition, ultra-thin two-dimension semiconductor material can be used as a kind of emerging energy-storage travelling wave tube, effect fast with charge/discharge speed
The advantages that rate is high, specific power is high, service life cycle is long and no pollution to the environment, therefore can be used as electric car and mixed type vapour
The energy-storage system of vehicle.
As a kind of photoelectric semiconductor material of rising in recent years, class graphite phase carbon nitride (g-C3N4) cause that people's is wide
General concern.g-C3N4Nano material due to excellent chemical stability, higher specific surface area, higher specific discharge capacity,
High rate performance and the abundant feature of structure species, are often used as conventional catalyst field green carriers and energy storage material.It is prior
It is to prepare g-C3N4Raw material it is cheap, abundance, pollution-free, this helps to produce in batches sexual valence than high catalysis material and light
Electric material promotes the commercialization of catalysis material and supercapacitor.However, most of g-C prepared by present3N4, compare table
There are also very big rooms for promotion for area, multiplying power behavior and cyclical stability, limit its more broad practice.
In short, forefathers are about g-C3N4Nanostructure is applied to gas sensor, catalysis material preparation and super capacitor
The report of electrode all absolutely proves g-C3N4The feasibility that material is applied in environment, energy field.Key problem is how to set
It counts, prepare the g-C with special construction3N4Nano material is to improve its specific surface area, multiplying power behavior and limited stable circulation
The performances such as property.There is also deficiencies for reported method, need optimization and improve.
Summary of the invention
It is an object of the invention to overcome defect of the existing technology, a kind of g-C is provided3N4Ultrathin nanometer chip architecture
Preparation method.
To achieve the goals above, The technical solution adopted by the invention is as follows:
G-C of the invention3N4The preparation method of ultrathin nanometer piece, comprising the following steps:
(1) melamine is dissolved in deionized water under water bath condition, stirring to melamine be dissolved completely in from
In sub- water, melamine aqueous solution is obtained；
(2) the melamine aqueous solution in step (1) is transferred to autoclave, carries out hydro-thermal reaction 12-24h；
(3) reactant obtained to the step (2) clean-centrifugal treating at least 3 times, cleaning-centrifugal treating step
Suddenly are as follows: deionized water is added in the reaction product or dehydrated alcohol cleans it, then carries out centrifugal treating, takes lower layer
Solids repeats cleaning-centrifugal treating step, and low temperature drying after cleaning-centrifugal treating obtains rodlike g-C3N4Forerunner
Object, and to g-C3N4Predecessor is ground；
(4) by the g-C after grinding in step (3)3N4Predecessor is made annealing treatment under nitrogen protection atmosphere, processing temperature
Degree is 400-500 DEG C, time 10-12h, and heating rate is 5-15 DEG C/min when processing, obtains g-C after annealing3N4
Ultrathin nanometer piece.
Preferably, melamine and the mass ratio of deionized water are 1-5:15-150 in the step (1).
Preferably, bath temperature is 70-95 DEG C in the step (1), water bath time 30-60min.
Preferably, in the step (2), the temperature of hydro-thermal reaction is 150-200 DEG C.
Preferably, in the step (3), the reactant that the step (2) obtains is handed over deionized water and dehydrated alcohol
For cleaning at least 3 times, and the revolving speed of centrifugal treating is not less than after cleaning every time
6000rpm, the time being centrifuged every time are 8-15min.
Preferably, in the step (3), when to reactant low temperature drying after cleaning up, reactant is placed in very
It is dried in empty drying box, control drying temperature is 60-80 DEG C, drying time 12-24h.
Preferably, in the step (4), to g-C3N4The time that predecessor is ground is no less than 30min.
The present invention is by adopting the above-described technical solution, have the advantages that
(1) preparation method of the present invention is simpler, successively using hydro-thermal reaction method and annealing method, during the preparation process zero
Pollution, no coupling product generate；
(2) the melamine amount that the present invention uses is few, at low cost, cheap and easy to get, and raw material is made full use of to carry out hydro-thermal
Synthesis, makes every effort to the best configuration of performance；
(3) the predecessor g-C in the present invention3N4Preparation be 70-95 DEG C water-bath carry out, it is simple and convenient, do not need
Expensive consersion unit, the reaction time is short, and repeatability is strong and yield is high, can be mass-produced；
(4) g-C prepared by the present invention3N4Ultrathin nanometer chip architecture has unique shape characteristic, for a large amount of few layer (3-5
Layer) shape stack made of two-dimensional ultrathin nanostructure, pattern is uniform and surface is smooth, can provide more activity and inhale
Attached site is conducive to the quick adsorption of organic pollutant molecule；Secondly, a large amount of nano flake stacks the structure to be formed greatly
Increase its specific surface area, and multiple-layer stacked structure can enhance its mechanical strength, the stability of its long-time service, the piece certainly will be improved
Shape ultra-thin materials all have good application prospect in terms of gas sensing, photochemical catalyst and catalyst carrier.
Detailed description of the invention
Fig. 1 is g-C prepared by embodiment 13N4The SEM of predecessor schemes；
Fig. 2 is g-C prepared by embodiment 13N4The SEM of ultrathin nanometer piece schemes；
Fig. 3 is g-C prepared by embodiment 13N4The XRD diagram of ultrathin nanometer piece.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention more comprehensible, preferred embodiment is enumerated below, to this hair
Bright further description.However, it is necessary to illustrate, many details listed in specification are used for the purpose of making reader to this
The one or more aspects of invention have a thorough explanation, also may be implemented even without these specific details of the invention
These aspects.
Embodiment 1
G-C of the invention3N4The preparation method of ultrathin nanometer piece, comprising the following steps:
(1) 1.0g melamine is added in 30mL deionized water, then their mixture is placed in 85 DEG C of constant temperature
30min is heated in water-bath, and stirs and is dissolved completely in deionized water to melamine, obtains melamine aqueous solution；
(2) the melamine aqueous solution in step (1) is transferred to autoclave, carries out hydro-thermal reaction, is lauched at 150 DEG C
Thermal response 12h, obtains reaction product；
(3) it is carried out after the reactant natural cooling that the step (2) obtains cleaning-centrifugal treating: using go from
1 progress centrifugal treating after sub- water or dehydrated alcohol clean it, the revolving speed of each centrifugal treating are 6000rpm, centrifugation
Time is 10min；Lower layer's solids is taken to repeat cleaning-centrifugal treating step to cleaning-centrifugal treating 6 times, when cleaning spends
Ionized water and dehydrated alcohol respectively clean 3 times, the lower layer's solids for taking cleaning-centrifugal treating to finish be placed in vacuum oven into
Row drying, control drying temperature are 80 DEG C, and drying time is for 24 hours, to obtain rodlike g-C3N4Predecessor, and by g-C3N4Forerunner
Object, which is placed in mortar, grinds 30min；
(4) by the g-C after grinding in step (3)3N4Predecessor is transferred in quartz boat, is moved back under nitrogen protection atmosphere
Fire processing, treatment temperature are 400 DEG C, time 10h, and heating rate is 10 DEG C/min when handling, with furnace after annealing
Natural cooling obtains g-C3N4Ultrathin nanometer piece.
Embodiment 2
G-C of the invention3N4The preparation method of ultrathin nanometer piece, comprising the following steps:
(1) 1.5g melamine is added in 30mL deionized water, then their mixture is placed in 70 DEG C of constant temperature
60min is heated in water-bath, and stirs and is dissolved completely in deionized water to melamine, obtains melamine aqueous solution；
(2) the melamine aqueous solution in step (1) is transferred to autoclave, carries out hydro-thermal reaction, is lauched at 200 DEG C
Thermal response 13.2h, obtains reaction product；
(3) it is carried out after the reactant natural cooling that the step (2) obtains cleaning-centrifugal treating: using go from
1 progress centrifugal treating after sub- water or dehydrated alcohol clean it, the revolving speed of each centrifugal treating are 6500rpm, centrifugation
Time is 8min；Take lower layer's solids to repeat cleaning-centrifugal treating step to cleaning-centrifugal treating 3 times, when cleaning spend from
Sub- water and dehydrated alcohol alternately clean, and the lower layer's solids for taking cleaning-centrifugal treating to finish is placed in vacuum oven and carries out
Dry, control drying temperature is 78 DEG C, and drying time 23h obtains rodlike g-C3N4Predecessor, and by g-C3N4Predecessor
It is placed in mortar and grinds 32min；
(4) by the g-C after grinding in step (3)3N4Predecessor is transferred in quartz boat, is moved back under nitrogen protection atmosphere
Fire processing, treatment temperature are 500 DEG C, time 12h, and heating rate is 15 DEG C/min when handling, with furnace after annealing
Natural cooling obtains g-C3N4The material of ultrathin nanometer chip architecture.
Embodiment 3
G-C of the invention3N4The preparation method of ultrathin nanometer piece, comprising the following steps:
(1) 2.0g melamine is added in 30mL deionized water, then their mixture is placed in 95 DEG C of constant temperature
35min is heated in water-bath, and stirs and is dissolved completely in deionized water to melamine, obtains melamine aqueous solution；
(2) the melamine aqueous solution in step (1) is transferred to autoclave, carries out hydro-thermal reaction, is lauched at 195 DEG C
Thermal response 14.5h, obtains reaction product；
(3) it is carried out after the reactant natural cooling that the step (2) obtains cleaning-centrifugal treating: using go from
1 progress centrifugal treating after sub- water or dehydrated alcohol clean it, the revolving speed of each centrifugal treating are 6600rpm, centrifugation
Time is 9min；Take lower layer's solids to repeat cleaning-centrifugal treating step to cleaning-centrifugal treating 4 times, when cleaning spend from
Sub- water and dehydrated alcohol alternately clean, and the lower layer's solids for taking cleaning-centrifugal treating to finish is placed in vacuum oven and carries out
Dry, control drying temperature is 75 DEG C, and drying time 21h obtains rodlike g-C3N4Predecessor, and by g-C3N4Predecessor
It is placed in mortar and grinds 35min；
(4) by the g-C after grinding in step (3)3N4Predecessor is transferred in quartz boat, is moved back under nitrogen protection atmosphere
Fire processing, treatment temperature are 495 DEG C, time 11.8h, and heating rate is 5 DEG C/min when handling, with furnace after annealing
Natural cooling obtains g-C3N4The material of ultrathin nanometer chip architecture.
Embodiment 4
G-C of the invention3N4The preparation method of ultrathin nanometer piece, comprising the following steps:
(1) 3.0g melamine is added in 450mL deionized water, then their mixture is placed in 92 DEG C of constant temperature
40min is heated in water-bath, and stirs and is dissolved completely in deionized water to melamine, obtains melamine aqueous solution；
(2) the melamine aqueous solution in step (1) is transferred to autoclave, carries out hydro-thermal reaction, is lauched at 190 DEG C
Thermal response 16h, obtains reaction product；
(3) it is carried out after the reactant natural cooling that the step (2) obtains cleaning-centrifugal treating: using go from
1 progress centrifugal treating after sub- water or dehydrated alcohol clean it, the revolving speed of each centrifugal treating are 6300rpm, centrifugation
Time is 11min；Lower layer's solids is taken to repeat cleaning-centrifugal treating step to cleaning-centrifugal treating 5 times, when cleaning spends
Ionized water and dehydrated alcohol alternately clean, the lower layer's solids for taking cleaning-centrifugal treating to finish be placed in vacuum oven into
Row drying, control drying temperature are 73 DEG C, and drying time 20h obtains rodlike g-C3N4Predecessor, and by g-C3N4Forerunner
Object, which is placed in mortar, grinds 36min；
(4) by the g-C after grinding in step (3)3N4Predecessor is transferred in quartz boat, is moved back under nitrogen protection atmosphere
Fire processing, treatment temperature are 490 DEG C, time 11.6h, and heating rate is 6 DEG C/min when handling, with furnace after annealing
Natural cooling obtains g-C3N4The material of ultrathin nanometer chip architecture.
Embodiment 5
G-C of the invention3N4The preparation method of ultrathin nanometer piece, comprising the following steps:
(1) 5.0g melamine is added in 750mL deionized water, then their mixture is placed in 90 DEG C of constant temperature
45min is heated in water-bath, and stirs and is dissolved completely in deionized water to melamine, obtains melamine aqueous solution；
(2) the melamine aqueous solution in step (1) is transferred to autoclave, carries out hydro-thermal reaction, is lauched at 186 DEG C
Thermal response 17h, obtains reaction product；
(3) it is carried out after the reactant natural cooling that the step (2) obtains cleaning-centrifugal treating: using go from
1 progress centrifugal treating after sub- water or dehydrated alcohol clean it, the revolving speed of each centrifugal treating are 6500rpm, centrifugation
Time is 11min；Lower layer's solids is taken to repeat cleaning-centrifugal treating step to cleaning-centrifugal treating 7 times, when cleaning spends
Ionized water and dehydrated alcohol alternately clean, the lower layer's solids for taking cleaning-centrifugal treating to finish be placed in vacuum oven into
Row drying, control drying temperature are 71 DEG C, and drying time 18h obtains rodlike g-C3N4Predecessor, and by g-C3N4Forerunner
Object, which is placed in mortar, grinds 37min；
(4) by the g-C after grinding in step (3)3N4Predecessor is transferred in quartz boat, is moved back under nitrogen protection atmosphere
Fire processing, treatment temperature are 480 DEG C, time 11.4h, and heating rate is 8 DEG C/min when handling, with furnace after annealing
Natural cooling obtains g-C3N4The material of ultrathin nanometer chip architecture.
Embodiment 6
G-C of the invention3N4The preparation method of ultrathin nanometer piece, comprising the following steps:
(1) 10.0g melamine is added in 1000mL deionized water, then their mixture is placed in 88 DEG C of perseverance
50min is heated in warm water bath, and stirs and is dissolved completely in deionized water to melamine, obtains melamine aqueous solution；
(2) the melamine aqueous solution in step (1) is transferred to autoclave, carries out hydro-thermal reaction, is lauched at 180 DEG C
Thermal response 18h, obtains reaction product；
(3) it is carried out after the reactant natural cooling that the step (2) obtains cleaning-centrifugal treating: using go from
1 progress centrifugal treating after sub- water or dehydrated alcohol clean it, the revolving speed of each centrifugal treating are 6800rpm, centrifugation
Time is 12min；Lower layer's solids is taken to repeat cleaning-centrifugal treating step to cleaning-centrifugal treating 4 times, when cleaning spends
Ionized water and dehydrated alcohol alternately clean, the lower layer's solids for taking cleaning-centrifugal treating to finish be placed in vacuum oven into
Row drying, control drying temperature are 60 DEG C, and drying time 12h obtains rodlike g-C3N4Predecessor, and by g-C3N4Forerunner
Object, which is placed in mortar, grinds 40min；
(4) by the g-C after grinding in step (3)3N4Predecessor is transferred in quartz boat, is moved back under nitrogen protection atmosphere
Fire processing, treatment temperature are 470 DEG C, time 11.1h, and heating rate is 9 DEG C/min when handling, with furnace after annealing
Natural cooling obtains g-C3N4The material of ultrathin nanometer chip architecture.
Embodiment 7
G-C of the invention3N4The preparation method of ultrathin nanometer piece, comprising the following steps:
(1) 15.0g melamine is added in 2000mL deionized water, then their mixture is placed in 82 DEG C of perseverance
55min is heated in warm water bath, and stirs and is dissolved completely in deionized water to melamine, obtains melamine aqueous solution；
(2) the melamine aqueous solution in step (1) is transferred to autoclave, carries out hydro-thermal reaction, is lauched at 170 DEG C
Thermal response 19h, obtains reaction product；
(3) it is carried out after the reactant natural cooling that the step (2) obtains cleaning-centrifugal treating: using go from
1 progress centrifugal treating after sub- water or dehydrated alcohol clean it, the revolving speed of each centrifugal treating are 7000rpm, centrifugation
Time is 12min；Lower layer's solids is taken to repeat cleaning-centrifugal treating step to cleaning-centrifugal treating 5 times, when cleaning spends
Ionized water and dehydrated alcohol alternately clean, the lower layer's solids for taking cleaning-centrifugal treating to finish be placed in vacuum oven into
Row drying, control drying temperature are 63 DEG C, and drying time 13.5h obtains rodlike g-C3N4Predecessor, and by g-C3N4Before
Drive object, which is placed in mortar, grinds 45min；
(4) by the g-C after grinding in step (3)3N4Predecessor is transferred in quartz boat, is moved back under nitrogen protection atmosphere
Fire processing, treatment temperature are 460 DEG C, time 11.3h, and heating rate is 11 DEG C/min when handling, after annealing with
Furnace natural cooling, obtains g-C3N4The material of ultrathin nanometer chip architecture.
Embodiment 8
G-C of the invention3N4The preparation method of ultrathin nanometer piece, comprising the following steps:
(1) 20.0g melamine is added in 2500mL deionized water, then their mixture is placed in 80 DEG C of perseverance
55min is heated in warm water bath, and stirs and is dissolved completely in deionized water to melamine, obtains melamine aqueous solution；
(2) the melamine aqueous solution in step (1) is transferred to autoclave, carries out hydro-thermal reaction, is lauched at 160 DEG C
Thermal response 21h, obtains reaction product；
(3) it is carried out after the reactant natural cooling that the step (2) obtains cleaning-centrifugal treating: using go from
1 progress centrifugal treating after sub- water or dehydrated alcohol clean it, the revolving speed of each centrifugal treating are 7200rpm, centrifugation
Time is 14min；Lower layer's solids is taken to repeat cleaning-centrifugal treating step to cleaning-centrifugal treating 6 times, when cleaning spends
Ionized water and dehydrated alcohol alternately clean, the lower layer's solids for taking cleaning-centrifugal treating to finish be placed in vacuum oven into
Row drying, control drying temperature are 66 DEG C, and drying time 18h obtains rodlike g-C3N4Predecessor, and by g-C3N4Forerunner
Object, which is placed in mortar, grinds 40min；
(4) by the g-C after grinding in step (3)3N4Predecessor is transferred in quartz boat, is moved back under nitrogen protection atmosphere
Fire processing, treatment temperature are 450 DEG C, time 11.5h, and heating rate is 12 DEG C/min when handling, after annealing with
Furnace natural cooling, obtains g-C3N4The material of ultrathin nanometer chip architecture.
Embodiment 9
G-C of the invention3N4The preparation method of ultrathin nanometer piece, comprising the following steps:
(1) 25.0g melamine is added in 3000mL deionized water, then their mixture is placed in 75 DEG C of perseverance
60min is heated in warm water bath, and stirs and is dissolved completely in deionized water to melamine, obtains melamine aqueous solution；
(2) the melamine aqueous solution in step (1) is transferred to autoclave, carries out hydro-thermal reaction, is lauched at 155 DEG C
Thermal response 23h, obtains reaction product；
(3) it is carried out after the reactant natural cooling that the step (2) obtains cleaning-centrifugal treating: using go from
1 progress centrifugal treating after sub- water or dehydrated alcohol clean it, the revolving speed of each centrifugal treating are 6000rpm, centrifugation
Time is 15min；Lower layer's solids is taken to repeat cleaning-centrifugal treating step to cleaning-centrifugal treating 5 times, when cleaning spends
Ionized water and dehydrated alcohol alternately clean, the lower layer's solids for taking cleaning-centrifugal treating to finish be placed in vacuum oven into
Row drying, control drying temperature are 68 DEG C, and drying time 14h obtains rodlike g-C3N4Predecessor, and by g-C3N4Forerunner
Object, which is placed in mortar, grinds 35min；
(4) by the g-C after grinding in step (3)3N4Predecessor is transferred in quartz boat, is moved back under nitrogen protection atmosphere
Fire processing, treatment temperature are 435 DEG C, time 11.8h, and heating rate is 13 DEG C/min when handling, after annealing with
Furnace natural cooling, obtains g-C3N4The material of ultrathin nanometer chip architecture.
Embodiment 10
G-C of the invention3N4The preparation method of ultrathin nanometer piece, comprising the following steps:
(1) 30.0g melamine is added in 3500mL deionized water, then their mixture is placed in 70 DEG C of perseverance
60min is heated in warm water bath, and stirs and is dissolved completely in deionized water to melamine, obtains melamine aqueous solution；
(2) the melamine aqueous solution in step (1) is transferred to autoclave, carries out hydro-thermal reaction, is lauched at 164 DEG C
Thermal response for 24 hours, obtains reaction product；
(3) it is carried out after the reactant natural cooling that the step (2) obtains cleaning-centrifugal treating: using go from
1 progress centrifugal treating after sub- water or dehydrated alcohol clean it, the revolving speed of each centrifugal treating are 6500rpm, centrifugation
Time is 10min；Lower layer's solids is taken to repeat cleaning-centrifugal treating step to cleaning-centrifugal treating 6 times, when cleaning spends
Ionized water and dehydrated alcohol alternately clean, the lower layer's solids for taking cleaning-centrifugal treating to finish be placed in vacuum oven into
Row drying, control drying temperature are 70 DEG C, and drying time 17h obtains rodlike g-C3N4Predecessor, and by g-C3N4Forerunner
Object, which is placed in mortar, grinds 50min；
(4) by the g-C after grinding in step (3)3N4Predecessor is transferred in quartz boat, is moved back under nitrogen protection atmosphere
Fire processing, treatment temperature are 450 DEG C, time 12h, and heating rate is 14 DEG C/min when handling, with furnace after annealing
Natural cooling obtains g-C3N4The material of ultrathin nanometer chip architecture.
Properties of product analysis
As shown in Figure 1-3, Fig. 1 is g-C obtained by 1 step of the present embodiment (2)3N4The stereoscan photograph of predecessor sample, from
The photo can be seen that g-C3N4The nano tube structure of single layer hollow, the g-C of this structure is presented in predecessor3N4Only have relatively
Small specific surface area.As seen from Figure 2, after making annealing treatment 10h in the nitrogen protection atmosphere at 400 DEG C, from the photo
It can be seen that g-C3N4Structure changes, and the folded nano flake structure of number layer heap, the g-C of this structure is presented3N4Specific surface area is aobvious
It writes and increases.Meanwhile XRD test is carried out to the product that annealing obtains, as shown in figure 3, its peak spectral line and g-C3N4Standard diffraction spectrum
The peak position of line is corresponding, it can be determined that prepared material is g-C3N4.The sample that 2-10 of the embodiment of the present invention is obtained is according to implementation
The detection method of example 1 is detected, after testing it is found that the present invention
The indices that sample is prepared in embodiment 2-10 are consistent with embodiment 1, herein without repeating.
Claims (7)
1. a kind of g-C3N4The preparation method of ultrathin nanometer piece, which is characterized in that the preparation method comprises the following steps:
(1) melamine is dissolved in deionized water under water bath condition, stirring to melamine is dissolved completely in deionized water
In, obtain melamine aqueous solution；
(2) the melamine aqueous solution in step (1) is transferred to autoclave, carries out hydro-thermal reaction 12-24h；
(3) reactant obtained to the step (2) carries out cleaning-centrifugal treating at least 3 times, cleaning-centrifugal treating step are as follows:
Deionized water is added in the reaction product or dehydrated alcohol cleans it, then carries out centrifugal treating, takes lower layer's solid
Object repeats cleaning-centrifugal treating step, and low temperature drying after cleaning-centrifugal treating obtains rodlike g-C3N4Predecessor,
And to g-C3N4Predecessor is ground；
(4) by the g-C after grinding in step (3)3N4Predecessor is made annealing treatment under nitrogen protection atmosphere, and treatment temperature is
400-500 DEG C, time 10-12h, and heating rate is 5-15 DEG C/min when processing, obtains g-C after annealing3N4It is ultra-thin
Nanometer sheet.
2. a kind of g-C according to claim 13N4The preparation method of ultrathin nanometer piece, which is characterized in that the step (1)
Middle melamine and the mass ratio of deionized water are 1-5:15-150.
3. a kind of g-C according to claim 13N4The preparation method of ultrathin nanometer piece, which is characterized in that the step (1)
Middle bath temperature is 70-95 DEG C, water bath time 30-60min.
4. a kind of g-C according to claim 13N4The preparation method of ultrathin nanometer piece, which is characterized in that the step (2)
In, the temperature of hydro-thermal reaction is 150-200 DEG C.
5. a kind of g-C according to claim 13N4The preparation method of ultrathin nanometer piece, which is characterized in that the step (3)
In, reactant alternately cleaning at least 3 times that the step (2) is obtained with deionized water and dehydrated alcohol, and every time after cleaning
The revolving speed of centrifugal treating is not less than 6000rpm, and the time being centrifuged every time is 8-15min.
6. a kind of g-C according to claim 13N4The preparation method of ultrathin nanometer piece, which is characterized in that the step (3)
In, when to reactant low temperature drying after cleaning up, reactant is placed in vacuum oven and is dried, controls drying
Temperature is 60-80 DEG C, drying time 12-24h.
7. a kind of g-C according to claim 13N4The preparation method of ultrathin nanometer piece, which is characterized in that the step (4)
In, to g-C3N4The time that predecessor is ground is no less than 30min.
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| CN111203262A (en) * | 2020-03-05 | 2020-05-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for rapidly preparing carbon nitride nanosheet loaded nano-copper, product and application thereof |
| CN112320771A (en) * | 2020-11-11 | 2021-02-05 | 深圳大学 | Thin-layer porous g-C prepared by supercritical water3N4Method (2) |
| CN112374473A (en) * | 2020-11-11 | 2021-02-19 | 深圳大学 | Phenol organic matter doped g-C synthesized based on phenol-containing wastewater3N4Method (2) |
| CN112897484A (en) * | 2021-01-14 | 2021-06-04 | 华南理工大学 | g-C without defect3N4Nanosheets, two-dimensional g-C3N4Nano sheet film, preparation method and application |
| CN114592197A (en) * | 2022-01-20 | 2022-06-07 | 华南理工大学 | Two-dimensional g-C3N4Nano-sheet membrane, electrochemical preparation method thereof and application thereof in ion separation |
| CN115196605A (en) * | 2022-05-19 | 2022-10-18 | 张家港市东大工业技术研究院 | Preparation method and application of graphite phase carbon nitride nanosheet |
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| CN112374473A (en) * | 2020-11-11 | 2021-02-19 | 深圳大学 | Phenol organic matter doped g-C synthesized based on phenol-containing wastewater3N4Method (2) |
| CN112897484A (en) * | 2021-01-14 | 2021-06-04 | 华南理工大学 | g-C without defect3N4Nanosheets, two-dimensional g-C3N4Nano sheet film, preparation method and application |
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| CN114592197A (en) * | 2022-01-20 | 2022-06-07 | 华南理工大学 | Two-dimensional g-C3N4Nano-sheet membrane, electrochemical preparation method thereof and application thereof in ion separation |
| CN115196605A (en) * | 2022-05-19 | 2022-10-18 | 张家港市东大工业技术研究院 | Preparation method and application of graphite phase carbon nitride nanosheet |
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Application publication date: 20190412 |