CN109569691A - Preparation method of boron doping carbonitride and products thereof and application - Google Patents
Preparation method of boron doping carbonitride and products thereof and application Download PDFInfo
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- CN109569691A CN109569691A CN201811576715.6A CN201811576715A CN109569691A CN 109569691 A CN109569691 A CN 109569691A CN 201811576715 A CN201811576715 A CN 201811576715A CN 109569691 A CN109569691 A CN 109569691A
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- boron doping
- carbonitride
- melamine
- boron
- doping carbonitride
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 29
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 29
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004327 boric acid Substances 0.000 claims abstract description 20
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 4
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000011175 product filtration Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 3
- 238000006731 degradation reaction Methods 0.000 claims description 3
- 239000004098 Tetracycline Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 229960002180 tetracycline Drugs 0.000 claims description 2
- 229930101283 tetracycline Natural products 0.000 claims description 2
- 235000019364 tetracycline Nutrition 0.000 claims description 2
- 150000003522 tetracyclines Chemical class 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 238000007146 photocatalysis Methods 0.000 abstract description 6
- 238000002156 mixing Methods 0.000 abstract description 4
- 241000446313 Lamella Species 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 206010054949 Metaplasia Diseases 0.000 abstract description 2
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical group [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 abstract description 2
- 230000002378 acidificating effect Effects 0.000 abstract description 2
- 230000003321 amplification Effects 0.000 abstract description 2
- 230000015689 metaplastic ossification Effects 0.000 abstract description 2
- 238000003199 nucleic acid amplification method Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- 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
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The present invention relates to preparation methods of a kind of boron doping carbonitride and products thereof and application, melamine and boric acid are carried out to the mode of hydro-thermal reaction, on the one hand promote boron atom and melamine that the mixing that chemical reaction makes boron and carbon nitrogen forms atomic level occurs, on the other hand hydro-thermal is carried out to melamine under acidic environment, a type supramolecular structure can be formed it into, the separation of carbonitride lamellar structure in subsequent roasting process is conducive to；Then the presoma by reaction synthesis roasts, and Uniform Doped, and the boron doping carbonitride that lamellar structure is thinner can be prepared.The boron doping carbonitride prepared using the method for the invention, element doping is uniform, and lamella is thinner, and photocatalysis performance is more preferable, and preparation manipulation is simple, and difficulty is lower, and amplification metaplasia is suitble to produce.
Description
Technical field
The invention belongs to field of nano material preparation, and in particular to a kind of preparation method and products thereof of boron doping carbonitride
And application.
Background technique
Energy crisis and environmental pollution are two Vital Strategic Problems faced in human social.With
Traditional fossil energy such as coal, petroleum, natural gas etc. increasingly depleted and in use bring a series of environmental problems,
The problem of effective use for clean energy resource, water, the purification of air and control field, seems urgent and important.Photocatalytic process
Solar energy can be changed into chemical energy, the decomposition to realize water, degradation, mineralising environment poison are reacted by photocatalytic redox
Element has many advantages, such as stable, efficient, pollution-free.It therefore, is the photocatalysis technology of core to being in economic society using catalysis material
Can make the transition the critical period China have particularly important meaning.
Polymer semiconductor's carbonitride has unique electronics knot as a kind of novel nonmetallic visible-light photocatalyst
Structure, visible light catalysis activity, chemistry and thermal stability are good, nontoxic and preparation is simple, are free of the features such as metal, but the light of carbonitride
It causes electron-hole pair recombination rate higher, its catalytic activity is caused to be restricted, therefore photochemical catalyst is carried out by mode appropriate
Modification improves photocatalytic activity, develops visible light-responded, efficient and stable catalysis material.
In order to improve this disadvantage, typically now improve its electronic structure and surface nature using the method for doping.Doping
Electronic structure is changed afterwards, and orbital hybridization occurs for doped chemical and the original molecular orbit of carbonitride, to change nitridation
The band structure of carbon, electronic structure and optical property.Have researches show that use boron doped carbonitride, the effect of photocatalysis hydrogen production
Rate can achieve undoped with preceding 4.3 times, and the ability with good degradating organic dye rhodamine B, and show good
Photostability.But currently used doping preparation method is usually to pass through solid phase for carbon nitride precursor and machine containing boron substance
It is prepared after tool mixing by roasting.Such as someone, using urea as presoma, tetraphenylboron sodium is doping boron source, passes through machinery
Then ball milling mixing roasts and boron doping carbonitride is prepared；Somebody using melamine as presoma, using sodium borohydride as
Preparation boron doping carbonitride is roasted after boron source and melamine mechanical mixture；The boron doping carbonitride prepared using these methods
The problem of uniform doping must be had, and further influence its photocatalysis performance.For example, someone is by the way of liquid phase doping
The carbonitride of boron doping more evenly is made, photocatalysis hydrogen production efficiency is using above-mentioned 2.5 simply adulterated times, this illustrates member
Element doping more evenly can further greatly improve hydrogen generation efficiency, but the mode of liquid phase doping recited above introduces other objects
On the one hand matter introduces impurity as surface charge modifying dose, another aspect element doping is also not especially uniformly, only relatively
More evenly in solid phase doping.
Summary of the invention
For existing preparation boron doping carbonitride, the non-uniform disadvantage of element doping, it is an object of that present invention to provide one kind
The preparation method of boron doping carbonitride.
Another object of the present invention is: providing a kind of boron doping nitridation carbon products of above method preparation.
Another object of the present invention is to: a kind of application of the said goods is provided.
The object of the invention is realized by following proposal: a kind of preparation method of boron doping carbonitride, by melamine and boron
Acid carries out hydro-thermal reaction, and then the presoma by reaction synthesis roasts, and Uniform Doped is prepared, and lamellar structure is thinner
Boron doping carbonitride, include the following steps:
1) melamine/boric acid/water 1:(0.01~1 in mass ratio): (5~100) weigh, first by melamine and boric acid with
And water is added in hydrothermal reaction kettle, is put into baking oven after stirring evenly and carries out hydro-thermal reaction, it is then that product filtration washing is true
Sky is drying to obtain presoma；
2) it will be put into crucible after presoma obtained above is ground, with 2.5 DEG C/min of heating in Muffle furnace
Rate is warming up to 400~600 DEG C, keeps the temperature 1~5 hour, obtained powder is boron doping carbonitride.
Mechanism of the present invention is: melamine and boric acid being carried out to the mode of hydro-thermal reaction, on the one hand promote boron atom and three
Poly cyanamid chemically reacts, and boron and carbon nitrogen is made to form the mixing of atomic level；On the other hand to three under acidic environment
Poly cyanamid carries out hydro-thermal, can form it into a type supramolecular structure, be conducive to carbonitride lamella knot in subsequent roasting process
The separation of structure.
The hydrothermal temperature is 100~200 DEG C, and the reaction time is 1~12 hour.
The present invention also provides a kind of boron doping carbonitrides, are prepared according to method described above.
Also, the present invention also provides a kind of boron doping carbonitride application of catalyst the most in tetracycline light degradation reaction.
Uniform Doped, and the boron doping carbonitride that lamellar structure is thinner can be prepared in the method for the invention, use
The boron doping carbonitride that the method for the present invention is prepared, element doping is uniform, and lamella is thinner, and photocatalysis performance is more preferable, and prepares
Easy to operate, difficulty is lower, and amplification metaplasia is suitble to produce.
Detailed description of the invention
The electron scanning micrograph of Fig. 1 boron doping carbonitride；
The distribution of boron element in Fig. 2 boron doping carbonitride.
Specific embodiment
The present invention is further illustrated below by embodiment, is not intended to limit the scope of the invention.
Embodiment 1
Melamine and boric acid are carried out hydro-thermal reaction by a kind of preparation method of boron doping carbonitride, then, by reaction synthesis
Presoma is roasted, and Uniform Doped, and the boron doping carbonitride that lamellar structure is thinner is prepared, includes the following steps:
Precise melamine, boric acid and water, wherein the mass ratio of melamine and boric acid be 1:0.1, melamine with
The mass ratio of water is 1:50, and first in melamine and boric acid and addition hydrothermal reaction kettle, baking oven is put into after stirring evenly
In, it is warming up to reaction a period of time (6 hours) after certain temperature (120 DEG C), is then by the vacuum drying of product filtration washing
Obtain presoma；
It is put into crucible and roasts after presoma is ground, heating rate is 2.5 DEG C/min, final calcination temperature
It is 500 DEG C, calcining time is 3 hours, and obtained powder is boron doping carbonitride.The scanning electron of product boron doping carbonitride
Microscope photo is shown in Fig. 1.Fig. 2 is shown in the distribution of boron element in boron doping carbonitride.
Embodiment 2
A kind of boron doping carbonitride, step is close with embodiment 1, prepares as follows:
Precise melamine, boric acid and water (wherein the mass ratio of melamine and boric acid is 1:0.3, melamine with
The mass ratio of water is 1:80), first in melamine and boric acid and addition hydrothermal reaction kettle, baking oven is put into after stirring evenly
In, it is warming up to reaction a period of time (5 hours) after certain temperature (180 DEG C), is then by the vacuum drying of product filtration washing
Obtain presoma；
It is put into crucible and is roasted that (wherein heating rate is 2.5 DEG C/min, final to roast after presoma is ground
Temperature is 550 DEG C, and calcining time is 4 hours), obtained powder is boron doping carbonitride.
Embodiment 3
A kind of boron doping carbonitride, step is close with embodiment 1, prepares as follows:
Precise melamine, boric acid and water (wherein the mass ratio of melamine and boric acid is 1:0.05, melamine with
The mass ratio of water is 1:80), first in melamine and boric acid and addition hydrothermal reaction kettle, baking oven is put into after stirring evenly
In, it is warming up to reaction a period of time (5 hours) after certain temperature (120 DEG C), is then by the vacuum drying of product filtration washing
Obtain presoma；
It is put into crucible and is roasted that (wherein heating rate is 2.5 DEG C/min, final to roast after presoma is ground
Temperature is 600 DEG C, and calcining time is 2 hours), obtained powder is boron doping carbonitride.
Embodiment 4
A kind of boron doping carbonitride, step is close with embodiment 1, prepares as follows:
Precise melamine, boric acid and water (wherein the mass ratio of melamine and boric acid is 1:0.1, melamine with
The mass ratio of water is 1:100), first in melamine and boric acid and addition hydrothermal reaction kettle, baking is put into after stirring evenly
In case, it is warming up to reaction a period of time (8 hours) after certain temperature (150 DEG C), is then dried in vacuo product filtration washing
Up to presoma；It is put into crucible and is roasted that (wherein heating rate is 2.5 DEG C/min, most after presoma is ground
Whole maturing temperature is 500 DEG C, and calcining time is 3 hours), obtained powder is boron doping carbonitride.Boron doping carbonitride
Each element content is seen attached list:
。
Claims (4)
1. a kind of preparation method of boron doping carbonitride, it is characterised in that melamine and boric acid are subjected to hydro-thermal reaction, then,
The presoma of reaction synthesis is roasted, Uniform Doped, and the boron doping carbonitride that lamellar structure is thinner is prepared, including
Following steps:
1) melamine/boric acid/water 1:(0.01~1 in mass ratio): (5~100) weigh, first by melamine and boric acid with
And water is added in hydrothermal reaction kettle, is put into baking oven after stirring evenly and carries out hydro-thermal reaction, it is then that product filtration washing is true
Sky is drying to obtain presoma；
2) it will be put into crucible after presoma obtained above is ground, with 2.5 DEG C/min of heating in Muffle furnace
Rate is warming up to 400~600 DEG C, keeps the temperature 1~5 hour, obtained powder is boron doping carbonitride.
2. the preparation method of boron doping carbonitride according to claim 1, which is characterized in that hydrothermal temperature 100
~200 DEG C, the reaction time is 1~12 hour.
3. a kind of boron doping carbonitride, it is characterised in that method according to claim 1 or claim 2 is prepared.
4. a kind of application of catalyst the most in tetracycline light degradation reaction of boron doping carbonitride according to claim 3.
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Cited By (14)
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| CN110064429A (en) * | 2019-05-31 | 2019-07-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of sulfur doping azotized carbon nano piece and products thereof and application |
| CN110433844A (en) * | 2019-08-08 | 2019-11-12 | 盐城工学院 | One kind containing Cr for efficient process6+(B, O) the codope g-C of waste water3N4The preparation method of photochemical catalyst |
| CN111085236A (en) * | 2019-12-30 | 2020-05-01 | 西北工业大学 | Preparation method of flexible recyclable photocatalytic film of carbon cloth loaded boron-doped graphite-phase carbon nitride |
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| CN111215113A (en) * | 2020-01-20 | 2020-06-02 | 暨南大学 | Iron-boron co-doped graphite-like phase carbon nitride photocatalyst and preparation method and application thereof |
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| CN112076738A (en) * | 2020-09-01 | 2020-12-15 | 齐鲁工业大学 | Boron-doped defective zinc oxide and preparation method and application thereof |
| CN112316970A (en) * | 2020-11-03 | 2021-02-05 | 陕西科技大学 | Preparation method and application of multi-defect graphite-phase carbon nitride photocatalyst |
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| CN115646530A (en) * | 2022-11-14 | 2023-01-31 | 吉林大学 | Double-promotion type boron-doped accordion-shaped graphite carbon nitride photocatalyst and preparation method and application thereof |
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Cited By (18)
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