CN107162048B - A kind of preparation method of titanium dioxide/nitridation carbon composite nano-material - Google Patents
A kind of preparation method of titanium dioxide/nitridation carbon composite nano-material Download PDFInfo
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- CN107162048B CN107162048B CN201710557954.6A CN201710557954A CN107162048B CN 107162048 B CN107162048 B CN 107162048B CN 201710557954 A CN201710557954 A CN 201710557954A CN 107162048 B CN107162048 B CN 107162048B
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 121
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 71
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 59
- 239000002131 composite material Substances 0.000 title claims abstract description 54
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- 238000005406 washing Methods 0.000 claims abstract description 25
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 21
- 239000000047 product Substances 0.000 claims abstract description 18
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 16
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 16
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000005642 Oleic acid Substances 0.000 claims abstract description 16
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 16
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 16
- 239000010936 titanium Substances 0.000 claims abstract description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 14
- 238000013019 agitation Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000010992 reflux Methods 0.000 claims abstract description 8
- 239000006228 supernatant Substances 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 230000001699 photocatalysis Effects 0.000 claims description 6
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 5
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 2
- LTUDISCZKZHRMJ-UHFFFAOYSA-N potassium;hydrate Chemical compound O.[K] LTUDISCZKZHRMJ-UHFFFAOYSA-N 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 description 21
- 238000000034 method Methods 0.000 description 9
- 239000002994 raw material Substances 0.000 description 7
- 230000001376 precipitating effect Effects 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- -1 amino, carbonyl Chemical group 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910001868 water Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical group [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 description 2
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- 238000011017 operating method Methods 0.000 description 2
- 238000006862 quantum yield reaction Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000004630 atomic force microscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000021615 conjugation Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
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- 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
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/671—Chalcogenides
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- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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Abstract
A kind of preparation method of titanium dioxide/nitridation carbon composite nano-material, comprising the following steps: S1:, which weighing, or measures carbon source, nitrogen source, oleic acid is added in three-necked flask；S2: installing and be heated to reflux device, under room temperature magnetic agitation by titanium source be added step S1 in three-necked flask in after carry out heating reaction, start timing when reaction system comes to life, after 10-50 minute stop heating and remove heat source；S3: after the reaction system cooled to room temperature after heating in step S2, supernatant liquid is removed, collects precipitated product；S4: the precipitated product obtained in step S3 is sufficiently washed, and the product after washing is 5-8 hours dry under 20-50 DEG C of vacuum condition；Dry to terminate to obtain titanium dioxide/nitridation carbon composite nano-material, the titanium dioxide/nitridation carbon composite nano-material is water-soluble titanium dioxide/nitridation carbon composite nano-material.The problem of preparation method of the present invention solves prior art operation complex steps, and time-consuming.
Description
[technical field]
The present invention relates to a kind of composite nano materials, and in particular to a kind of titanium dioxide/nitridation carbon composite nano-material
Preparation method.
[background technique]
Time-consuming for the preparation method of current most of titanium dioxide/nitridation carbon composite nano-material, cumbersome, Bu Nengman
The requirement that foot simplicity is quickly prepared.Traditional preparation method is titanium source to be first passed through to reaction titanium hydroxide (Ti (OH) is made4) or
Titanium dioxide, and the substance with nitridation carbon structure is made in carbon source, nitrogen source reaction, then by titanium hydroxide obtained or titanium dioxide
Titanium calcines obtained titanium dioxide/nitridation carbon composite with the substance with nitridation carbon structure, and overall flow is complex for operation step,
Time-consuming is tens hours.
[summary of the invention]
To solve the above-mentioned problems, the present invention provides a kind of preparation method of titanium dioxide/nitridation carbon composite nano-material,
Largely shorten the time of material preparation and simplify operating procedure, realizes that simple and efficient to prepare titanium dioxide/carbonitride multiple
The problem of purpose for closing nano material, solves prior art operation complex steps, and time-consuming.
The present invention is achieved by the following technical solutions, provides a kind of titanium dioxide/nitridation carbon composite nano-material
Preparation method, comprising the following steps:
S1:, which weighing, or measures carbon source, nitrogen source, oleic acid is added in three-necked flask, the carbon source, nitrogen source, oleic acid additional amount
Depending on carbon source, the ratio of 1 gram of nitrogen source total weight addition, 10 milliliters of oleic acid, it is ensured that carbon source, nitrogen source can be completely dissolved, wherein carbon
Source, the additional amount of nitrogen source are equal；
S2: installing and be heated to reflux device, and 0.5-2.5 milliliters of titanium sources are added in step S1 under room temperature magnetic agitation
In three-necked flask, setting temperature is 100-220 DEG C and carries out heating reaction, if temperature is lower than 100 DEG C at this time, raw material is not readily dissolved,
If temperature is higher than 220 DEG C, material is easy carbonization and poorly water-soluble, starts timing when reaction system comes to life, 10-50 minutes
Stop heating afterwards and remove heat source, if the reaction time, raw material reaction was insufficient, and resulting materials may not have lower than 10 minutes at this time
Standby photoluminescent property, if the reaction time is more than 50 minutes, resulting materials carbonization is serious and poorly water-soluble even loses photoluminescent property；In
For preparing water soluble fluorescence composite material in this step, titanium source is added to be advisable with 0.5 milliliter, and it is glimmering to improve to a certain degree material
Quantum yield, but should not be added excessively, fluorescence quantum yield is otherwise reduced instead；For preparing water-insoluble catalysis material,
Titanium source is added to be advisable with 2.5 milliliters, and the accounting raising of titanium source can improve composite material catalytic effect, but addition titanium source is excessive, then
There are problems that causing experiment safety because excessive titanium source hydrolyzes acutely；
S3: after the reaction system cooled to room temperature after heating in step S2, removing supernatant liquid, collects precipitating and produces
Object；
S4: the precipitated product obtained in step S3 is first washed 3-6 times with n-hexane, if insufficient lower than 3 washings, 6
Secondary can guarantee washes away the organic phases substance such as oleic acid, and detergent and waste of time, each wash time are then caused more than 6 times
15-20 seconds, the time was too short, failed sufficiently to wash, too long, wasted time；Again with anhydrous second after n-hexane sufficiently washs for use
Alcohol washs 1-3 times, because material polarity is larger, there is certain dissolubility in dehydrated alcohol, according to the dissolution situation of different materials,
Select washing times and not exceeding 3 times as one sees fit, every time washing 5-10 second, number it is too low it is too short with the time cannot be by residual raw materials
It cleans, it is excessively high and too long, cause material loss；Product after washing is 5-8 hours dry under 20-50 DEG C of vacuum condition, if
Temperature is too low, needs the dry time that will extend and causes waste of time, may make material remnants' if temperature is excessively high
It is chemically reacted in the presence of dehydrated alcohol；It is dry to terminate to obtain titanium dioxide/nitridation carbon composite nano-material, the titanium dioxide
Titanium/nitridation carbon composite nano-material is water-soluble titanium dioxide/nitridation carbon composite nano-material.
Particularly, further comprising the steps of:
S5: water-soluble titanium dioxide made from step S4/nitridation carbon composite nano-material is placed in ceramic crucible, is put into
Muffle furnace is calcined 1-3 hours, and the water-insoluble titanium dioxide with photocatalytic performance/nitridation carbon composite nano material is made
Material；If calcination time is too short in this step, material fails to form the more regular graphite phase carbon nitride of lattice and titanium dioxide, too long
Then it is ashed carbonitride.
Particularly, the carbon source in the step S1 is monohydrate potassium, tartaric acid, glucose, these raw materials are heating
Under the conditions of dissolve in oleic acid, and be rich in carboxyl or hydroxyl, the substance of generation nitrogen carbon structure can react with common nitrogen source.
Particularly, the nitrogen source in the step S1 is urea, ethylenediamine, melamine, these raw materials are in a heated condition
Oleic acid is dissolved in, and is rich in nitrogen, the substance for generating nitrogen carbon structure can be reacted with common carbon source.
Particularly, the titanium source in the step S2 is butyl titanate, and butyl titanate is common titanium source, can be dissolved in most organic
Solvent, dissolubility is preferable in oleic acid.
The beneficial effects of the invention are as follows utilize hydroxyl, amino, carbonyl, the substitution of carboxylic acid compound, cyclization in Organic Ingredients
The generations such as substitution reaction of aromatic ring conjugation is even crosslinked and is similar to the structure of carbonitride in reaction and raw material.Meanwhile it is former
The crystallization water in material is conducive to butyl titanate hydrolysis and generates the titanium dioxide intermediates such as titanium hydroxide and react final by heating
Titanium dioxide is generated in the composite.Since one-step method is from carbon source, nitrogen source, the reaction jointly of three raw material of titanium source, avoid passing
System method first prepares after titanium dioxide or titanium dioxide intermediate, carbonitride the multi-step of compound preparation and cumbersome behaviour again respectively
Make, thus greatly shortens preparation time and simplify operating procedure.Material made from one-step method after high-temperature calcination, hydroxyl, carbonyl,
Amino groups are separately converted to the volatilization of the substances such as water, carbon dioxide, ammonia, to realize more regular graphite phase carbon nitride
It is carried out with titanium dioxide compound.
[Detailed description of the invention]
Fig. 1 is water-soluble titanium dioxide produced by the present invention/nitridation carbon composite nano-material transmission electron microscope figure
(A)；
Fig. 2 is water-soluble titanium dioxide produced by the present invention/nitridation carbon composite nano-material atomic force microscopy diagram
(B)；
Fig. 3 is the transmission electron microscope of water-insoluble titanium dioxide/nitridation carbon composite nano-material produced by the present invention
Scheme (A)；
Fig. 4 is the high-resolution transmitted electron of water-insoluble titanium dioxide/nitridation carbon composite nano-material produced by the present invention
Microscope figure.
[specific embodiment]
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below by way of specific embodiment to this
Invention is described in detail.
Embodiment 1:
A method of water-soluble titanium dioxide/nitridation carbon composite nano-material is prepared, is made using following steps:
S1:, which weighing, or measures 2 grams of carbon sources, 2 grams of nitrogen sources, 40 milliliters of oleic acid is added in three-necked flask；
S2: installing and be heated to reflux device, and 0.5 milliliter of butyl titanate is added in step S1 under room temperature magnetic agitation
In three-necked flask, setting temperature is 180 DEG C and carries out heating reaction, starts timing when reaction system comes to life, after 30 minutes
Stop heating and removes heat source；
S3: after the reaction system cooled to room temperature after heating in step S2, removing supernatant liquid, collects precipitating and produces
Object；
S4: the precipitated product obtained in step S3 is first washed 3 times with n-hexane, each wash time 20 seconds；For use just
Hexane is washed 3 times with dehydrated alcohol again after sufficiently washing, every time washing 5 seconds；By the product after washing under 50 DEG C of vacuum conditions
It is 8 hours dry；It is dry to terminate to obtain water-soluble titanium dioxide/nitridation carbon composite nano-material.
Embodiment 2:
A method of water-soluble titanium dioxide/nitridation carbon composite nano-material is prepared, is made using following steps:
S1:, which weighing, or measures 2 grams of carbon sources, 2 grams of nitrogen sources, 40 milliliters of oleic acid is added in three-necked flask；
S2: installing and be heated to reflux device, and 2.5 milliliters of butyl titanates are added in step S1 under room temperature magnetic agitation
In three-necked flask, setting temperature is 220 DEG C and carries out heating reaction, starts timing when reaction system comes to life, after ten minutes
Stop heating and removes heat source；
S3: after the reaction system cooled to room temperature after heating in step S2, removing supernatant liquid, collects precipitating and produces
Object；
S4: the precipitated product obtained in step S3 is first washed 6 times with n-hexane, each wash time 15 seconds；For use just
Hexane is washed 1 time with dehydrated alcohol again after sufficiently washing, every time washing 10 seconds；By the product after washing under 20 DEG C of vacuum conditions
It is 6 hours dry；It is dry to terminate to obtain water-soluble titanium dioxide/nitridation carbon composite nano-material.
Embodiment 3:
A method of water-soluble titanium dioxide/nitridation carbon composite nano-material is prepared, is made using following steps:
S1:, which weighing, or measures 1.5 grams of carbon sources, 1.5 grams of nitrogen sources, 30 milliliters of oleic acid is added in three-necked flask；
S2: installing and be heated to reflux device, and three in step S1 are added in 2 milliliters of butyl titanates under room temperature magnetic agitation
In mouth flask, setting temperature is 100 DEG C and carries out heating reaction, starts timing when reaction system comes to life, stops after 50 minutes
It only heats and removes heat source；
S3: after the reaction system cooled to room temperature after heating in step S2, removing supernatant liquid, collects precipitating and produces
Object；
S4: the precipitated product obtained in step S3 is first washed 4 times with n-hexane, each wash time 17 seconds；For use just
Hexane is washed 2 times with dehydrated alcohol again after sufficiently washing, every time washing 7 seconds；By the product after washing under 30 DEG C of vacuum conditions
It is 6 hours dry；It is dry to terminate to obtain water-soluble titanium dioxide/nitridation carbon composite nano-material；
S5: water-soluble titanium dioxide made from step S4/nitridation carbon composite nano-material is placed in ceramic crucible, is put into
Muffle furnace is calcined 1 hour, and the water-insoluble titanium dioxide with photocatalytic performance/nitridation carbon composite nano-material is made.
Embodiment 4:
A method of water-soluble titanium dioxide/nitridation carbon composite nano-material is prepared, is made using following steps:
S1:, which weighing, or measures 1.2 grams of carbon sources, 1.2 grams of nitrogen sources, 24 milliliters of oleic acid is added in three-necked flask；
S2: installing and be heated to reflux device, and 2.2 milliliters of butyl titanates are added in step S1 under room temperature magnetic agitation
In three-necked flask, setting temperature is 200 DEG C and carries out heating reaction, starts timing when reaction system comes to life, after forty minutes
Stop heating and removes heat source；
S3: after the reaction system cooled to room temperature after heating in step S2, removing supernatant liquid, collects precipitating and produces
Object；
S4: the precipitated product obtained in step S3 is first washed 5 times with n-hexane, each wash time 16 seconds；For use just
Hexane is washed 2 times with dehydrated alcohol again after sufficiently washing, every time washing 9 seconds；By the product after washing under 40 DEG C of vacuum conditions
It is 7 hours dry；It is dry to terminate to obtain water-soluble titanium dioxide/nitridation carbon composite nano-material；
S5: water-soluble titanium dioxide made from step S4/nitridation carbon composite nano-material is placed in ceramic crucible, is put into
Muffle furnace is calcined 3 hours, and the water-insoluble titanium dioxide with photocatalytic performance/nitridation carbon composite nano-material is made.
Embodiment 5:
A method of water-insoluble titanium dioxide/nitridation carbon composite nano-material being prepared, using following steps production
At:
S1:, which weighing, or measures 2 grams of carbon sources, 2 grams of nitrogen sources, 40 milliliters of oleic acid is added in three-necked flask；
S2: installing and be heated to reflux device, and 2.5 milliliters of butyl titanates are added in step S1 under room temperature magnetic agitation
In three-necked flask, setting temperature is 180 DEG C and carries out heating reaction, starts timing when reaction system comes to life, after 30 minutes
Stop heating and removes heat source；
S3: after the reaction system cooled to room temperature after heating in step S2, removing supernatant liquid, collects precipitating and produces
Object；
S4: the precipitated product obtained in step S3 is first washed 3 times with n-hexane, each wash time 20 seconds；For use just
Hexane is washed 3 times with dehydrated alcohol again after sufficiently washing, every time washing 5 seconds；By the product after washing under 50 DEG C of vacuum conditions
It is 8 hours dry；It is dry to terminate to obtain water-soluble titanium dioxide/nitridation carbon composite nano-material.
S5: water-soluble titanium dioxide made from step S4/nitridation carbon composite nano-material is placed in ceramic crucible, is put into
It is calcined 2 hours at 550 DEG C in Muffle furnace, the titanium dioxide/carbonitride with photocatalytic performance for being made water-insoluble is multiple
Close nano material.
In the embodiment of the present invention, the wherein made water-soluble titanium dioxide of embodiment 1/nitridation carbon composite nano-material fluorescence volume
Sub- yield is higher with respect to other embodiments, can ensure that sufficiently washing, reduces washing loss, is sufficiently dry and time-consuming moderate.
The made water-insoluble titanium dioxide of embodiment 5/nitridation carbon composite nano-material catalytic effect is with respect to other embodiments
It is good, it can guarantee experiment safety while obtaining preferable catalytic effect, and time-consuming moderate.
As Fig. 1 and Fig. 2 it is found that water-soluble titanium dioxide made from embodiment 1 and embodiment 2/nitridation carbon composite nano material
Material is in nano-sheet, X-ray diffraction spectra, Fourier transform infrared spectroscopy, the height of comprehensive analysis material in size and shape
Differentiating x-ray photoelectron spectroscopy figure may infer that the water-soluble titanium dioxide/nitridation carbon composite nano-material is functionalized two
Titanium oxide/azotized carbon nano piece.Materials show fluorescent characteristic has potential application in hypochlorous acid detection.
Water-insoluble titanium dioxide/carbonitride with photocatalytic performance is compound made from 3 embodiment 4 of embodiment receives
Rice material further confirms that the material is titanium dioxide in conjunction with Fig. 3 and Fig. 4 comprising anatase titania and graphite phase carbon nitride
Titanium/nitridation carbon composite nano-material.The degradation of the significantly accelerated methylene blue of energy under visible light is added in the material, illustrates this
Potential using value of the material in terms of environment water pollution control.
It should be understood that it can be modified or changed according to the above description for those skilled in the art, and
All these modifications and variations should all belong to the protection domain of appended claims of the present invention.
Claims (5)
1. a kind of titanium dioxide/nitridation carbon composite nano-material preparation method, which comprises the following steps:
S1:, which weighing, or measures carbon source, nitrogen source, oleic acid is added in three-necked flask, and the carbon source, nitrogen source, oleic acid additional amount press carbon
Source, 1 gram of nitrogen source total weight addition 10 milliliters of oleic acid ratio depending on, wherein carbon source, the additional amount of nitrogen source are equal；
S2: installing and be heated to reflux device, and three mouthfuls in step S1 are added in 0.5-2.5 milliliters of titanium sources under room temperature magnetic agitation
In flask, setting temperature is 100-220 DEG C and carries out heating reaction, starts timing when reaction system comes to life, 10-50 minutes
Stop heating afterwards and removes heat source；
S3: after the reaction system cooled to room temperature after heating in step S2, supernatant liquid is removed, collects precipitated product；
S4: the precipitated product obtained in step S3 is first washed 3-6 times with n-hexane, and each wash time 15-20 seconds；For use just
Hexane is washed 1-3 times with dehydrated alcohol again after sufficiently washing, every time washing 5-10 seconds；Product after washing is true at 20-50 DEG C
It is 5-8 hours dry under empty condition；It is dry to terminate to obtain titanium dioxide/nitridation carbon composite nano-material, the titanium dioxide/nitridation
Carbon composite nano-material is water-soluble titanium dioxide/nitridation carbon composite nano-material.
2. a kind of preparation method of titanium dioxide/nitridation carbon composite nano-material according to claim 1, feature exist
In further comprising the steps of:
S5: water-soluble titanium dioxide made from step S4/nitridation carbon composite nano-material is placed in ceramic crucible, Muffle is put into
Furnace is calcined 1-3 hours, and the water-insoluble titanium dioxide with photocatalytic performance/nitridation carbon composite nano-material is made.
3. a kind of preparation method of titanium dioxide/nitridation carbon composite nano-material according to claim 1, feature exist
In the carbon source in the step S1 is monohydrate potassium, tartaric acid, glucose.
4. a kind of preparation method of titanium dioxide/nitridation carbon composite nano-material according to claim 1, feature exist
In the nitrogen source in the step S1 is urea, ethylenediamine, melamine.
5. a kind of preparation method of titanium dioxide/nitridation carbon composite nano-material according to claim 1, feature exist
In the titanium source in the step S2 is butyl titanate.
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