CN104108687A - Carbon nitride and preparation method thereof - Google Patents
Carbon nitride and preparation method thereof Download PDFInfo
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- CN104108687A CN104108687A CN201410361328.6A CN201410361328A CN104108687A CN 104108687 A CN104108687 A CN 104108687A CN 201410361328 A CN201410361328 A CN 201410361328A CN 104108687 A CN104108687 A CN 104108687A
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Abstract
The invention discloses a preparation method of carbon nitride, which comprises the following step: carrying out high-temperature annealing on 5-azacytosine in a non-oxidizing atmosphere to prepare the carbon nitride, wherein the heating rate is 0.2-10 DEG C/minute, the annealing temperature is 400-700 DEG C, and the annealing time is 2-8 hours. The method can be used for preparing the high-specific-area carbon nitride material under the condition of no template, and thus, has the advantages of simplified technique, no template, one-step preparation and the like.
Description
Technical field
The present invention relates to function nano technical field, relate in particular to a kind of carbonitride and preparation method thereof.
Background technology
Carbonitride, due to its unique physical structure and electronic band structure, is subject to extensive concern in fields such as photochemical catalysis, energy transformation, electrocatalysis, drug delivery, support of the catalyst, solar cells.Traditional to pass through the carbonitride specific surface area that the thermal polycondensation methods such as nitrile amine, dicyanamide, trimeric cyanamide make little, restricted the application of carbonitride in above-mentioned field.By changing the nanometer particle size of carbonitride and pattern, increase its specific surface area and can improve its actual application performance.At present, although adjusting process or adopt template prepared a series of different-shapes carbonitride quantum dot, nano wire, nanotube,, nanometer rod, nano particle, nanometer ball, nano-cluster etc., there is complex steps, the shortcoming such as time-consuming.
Summary of the invention
Technical problem to be solved by this invention is: a kind of method of preparing the carbonitride of high-ratio surface is provided.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
A preparation method for carbonitride, by 5-nitrogen cytosine high temperature annealing in nonoxidizing atmosphere, makes carbonitride, and wherein temperature rise rate is: 0.2-10 ℃/min, annealing temperature is: 400-700 degree, annealing time is: 2-8 hour.
In order to solve the problems of the technologies described above, another technical solution used in the present invention is:
A preparation method for carbonitride, comprises the following steps:
1) precursor preparation: 5-nitrogen cytosine and 2,5-, bis-sulphur two ureas in mass ratio example are 3:1-5:1, or 5-nitrogen cytosine is routine for 3:1-5:1 mixes in mass ratio with amidinothiourea, and the mixture of formation is precursor;
2) high temperature annealing: by precursor high temperature annealing in nonoxidizing atmosphere, make carbonitride, wherein temperature rise rate is: 0.2-10 ℃/min, annealing temperature is: 400-700 degree, annealing time is: 2-8 hour.
Beneficial effect of the present invention is: by preparing the carbon nitride material of high-ratio surface under the condition without template.The method has technique and simplifies, without template, single stage method, the advantage such as prepares.
Accompanying drawing explanation
Fig. 1 is the SEM figure () of the carbonitride of the embodiment of the present invention 1 preparation.
Embodiment
By describing technology contents of the present invention, structural attitude in detail, being realized object and effect, below in conjunction with embodiment and coordinate accompanying drawing to be explained in detail.
The design of most critical of the present invention is: select suitable precursor and prepare by pyrocondensation method the carbonitride that a kind of specific surface area is large, the method technique is simplified, without template, single stage method, prepared etc.
carbonitride: the carbonitride that pattern is, carbonitride (β-C
3n
4) be that a kind of hardness can compare favourably with diamond and at occurring in nature undiscovered new covalent compound still.
5-nitrogen cytosine: Chinese another name: 5-nitrogen cytosine, 5-azepine cytosine(Cyt), 4-amino-1,3,5-triazines-2-ketone, English name: 5-Azacytosine, purity:>=98% (HPLC), molecular formula: C
3h
4n
4o.
2,5-, bis-sulphur two ureas: white to off-white color crystalline powder bis-thiourea is the intermediate of sterilant bismerthiazol.Hydrazonium sulfate and thiocyanic acid amine through condensation, reset out.Its preparation method is under stirring, to drop into wet basis hydrazonium sulfate in reactor, adds catalyzer a small amount of, and then drops into ammonium thiocyanate, opens jacket steam reflux 3.5h, cooling, and blowing filters, and washes with water, and vacuum suction filter, to dry, obtains finished product.
amidinothiourea: itself there is anti-hypoxia active, as medicine famotidine intermediate, with Dyhard RU 100, p-benzoqui(o)none dioxime, hydrogen sulfide reaction, make.Chinese another name: amidinothiourea, guarana seed extract, carbonamidine thiocarbamide, 2-imino--4-sulfuration biuret, amidinothiourea.
The preparation method of carbonitride of the present invention mainly contains two kinds of first and uses separately 5-nitrogen cytosine for precursor, another kind is 5-nitrogen cytosine and 2,5-bis-sulphur two ureas in mass ratio example are 3:1-5:1, or 5-nitrogen cytosine and amidinothiourea in mass ratio example mix as precursor for 3:1-5:1, by precursor high temperature annealing in nonoxidizing atmosphere, make carbonitride, wherein temperature rise rate is: 0.2-10 ℃/min, annealing temperature is: 400-700 degree, annealing time is: 2-8 hour.
Embodiment 1
Embodiment 1, takes 2 grams of 5-nitrogen cytosines, puts it in magnetic boat, then with tube furnace, heats by the speed of 0. ℃/min and heat up in nitrogen, 500 degree heating 2 hours, can obtain carbonitride.Fig. 1 is the stereoscan photograph of the carbonitride prepared of the present embodiment.As shown in Figure 1, Graphene surface arrangement has uniform hole, and the diameter of porous graphene is nm left and right.
Embodiment 2, take 2 grams of 5-nitrogen cytosines, put it in magnetic boat, then with tube furnace, heat by the speed of 10 ℃/min and heat up in nitrogen, 500 degree heating 2 hours, can obtain carbonitride.
Embodiment 3, take 2 grams of 5-nitrogen cytosines, put it in magnetic boat, then with tube furnace, heat by the speed of 2 ℃/min and heat up in nitrogen, 700 degree heating 2 hours, can obtain carbonitride.
Embodiment 4, take 3 grams of 5-nitrogen cytosines and 1 gram of two sulphur two urea, after it is fully mixed, put into magnetic boat, then with tube furnace, heat by the speed of 5 ℃/min and heat up in nitrogen, 500 degree heating 2 hours, can obtain carbonitride.
Embodiment 5, take 2.5 grams of 5-nitrogen cytosines and 0.5 gram of amidinothiourea, after it is fully mixed, put into magnetic boat, then with tube furnace, heat by the speed of 5 ℃/min and heat up in nitrogen, 500 degree heating 2 hours, can obtain carbonitride.
Embodiment 6, take 2.5 grams of 5-nitrogen cytosines and 0.5 gram of two sulphur two urea, after it is fully mixed, put into magnetic boat, then with tube furnace, heat by the speed of 5 ℃/min and heat up in argon gas, 500 degree heating 2 hours, can obtain carbonitride.
Embodiment 7, take 3 grams of 5-nitrogen cytosines and 1 gram of amidinothiourea, after it is fully mixed, put into magnetic boat, then with tube furnace, heat by the speed of 5 ℃/min and heat up in ammonia, 500 degree heating 2 hours, can obtain carbonitride.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes specification sheets of the present invention and accompanying drawing content to do; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (6)
1. a preparation method for carbonitride, is characterized in that, by 5-nitrogen cytosine high temperature annealing in nonoxidizing atmosphere, makes carbonitride, and wherein temperature rise rate is: 0.2-10 ℃/min, annealing temperature is: 400-700 degree, annealing time is: 2-8 hour.
2. the preparation method of carbonitride according to claim 1, is characterized in that, takes 2 grams of 5-nitrogen cytosines, put it in magnetic boat, then with tube furnace, in nitrogen, heat the speed intensification of pressing 0.2-2 ℃/min, 500 degree heating 2 hours, can obtain carbonitride.
3. the preparation method of carbonitride according to claim 1, is characterized in that, takes 2 grams of 5-nitrogen cytosines, put it in magnetic boat, then with tube furnace, in nitrogen, heat the speed intensification of pressing 5-10 ℃/min, 500 degree heating 2 hours, can obtain carbonitride.
4. a preparation method for carbonitride, is characterized in that, comprises the following steps:
1) precursor preparation: 5-nitrogen cytosine and 2,5-, bis-sulphur two ureas in mass ratio example are 3:1-5:1, or 5-nitrogen cytosine is routine for 3:1-5:1 mixes in mass ratio with amidinothiourea, and the mixture of formation is precursor;
2) high temperature annealing: by precursor high temperature annealing in nonoxidizing atmosphere, make carbonitride, wherein temperature rise rate is: 0.2-10 ℃/min, annealing temperature is: 400-700 degree, annealing time is: 2-8 hour.
5. the preparation method of carbonitride according to claim 4, is characterized in that step 2) in precursor is put into magnetic boat, then with tube furnace, in nitrogen, heat the speed intensification of press 2-5 ℃/min, at 500 degree, heat 2-5 hour.
6. the carbonitride preparing according to the preparation method described in claim 1-5 any one.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106902859A (en) * | 2017-03-21 | 2017-06-30 | 江苏理工学院 | A kind of efficient carbon auto-dope graphite phase carbon nitride visible light catalyst and its preparation method and application |
| CN113786855A (en) * | 2021-09-23 | 2021-12-14 | 黑龙江大学 | Carbon nitride-Pd nano particle material and preparation method and application thereof |
| CN114100665A (en) * | 2021-12-06 | 2022-03-01 | 合肥工业大学 | Preparation method and application of carbonyl functionalized graphite phase carbon nitride |
| CN114588937A (en) * | 2022-03-16 | 2022-06-07 | 浙江大学 | Preparation method and application of pyridazine-doped modified C3N4 photocatalyst |
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| CN101323437A (en) * | 2008-07-25 | 2008-12-17 | 中北大学 | Explosion impact synthetic method of beta-C3N4 |
| CN103145108A (en) * | 2013-02-07 | 2013-06-12 | 重庆工商大学 | Preparation method of C3N4 organic heterojunction |
| CN103539090A (en) * | 2013-10-30 | 2014-01-29 | 吉林大学 | High orientation arrayed carbon nitride nanorod array and preparation method thereof |
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| CN101323437A (en) * | 2008-07-25 | 2008-12-17 | 中北大学 | Explosion impact synthetic method of beta-C3N4 |
| CN103145108A (en) * | 2013-02-07 | 2013-06-12 | 重庆工商大学 | Preparation method of C3N4 organic heterojunction |
| CN103539090A (en) * | 2013-10-30 | 2014-01-29 | 吉林大学 | High orientation arrayed carbon nitride nanorod array and preparation method thereof |
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| R. ALEXANDRESCU,ET AL.: "Preparation of carbon nitride fine powder by laser induced gas-phase reactions", 《APPL. PHYS. A》 * |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106902859A (en) * | 2017-03-21 | 2017-06-30 | 江苏理工学院 | A kind of efficient carbon auto-dope graphite phase carbon nitride visible light catalyst and its preparation method and application |
| CN113786855A (en) * | 2021-09-23 | 2021-12-14 | 黑龙江大学 | Carbon nitride-Pd nano particle material and preparation method and application thereof |
| CN113786855B (en) * | 2021-09-23 | 2024-03-19 | 黑龙江大学 | Carbon nitride-Pd nanoparticle material and preparation method and application thereof |
| CN114100665A (en) * | 2021-12-06 | 2022-03-01 | 合肥工业大学 | Preparation method and application of carbonyl functionalized graphite phase carbon nitride |
| CN114100665B (en) * | 2021-12-06 | 2024-03-29 | 合肥工业大学 | Preparation method and application of carbonyl functionalized graphite phase carbon nitride |
| CN114588937A (en) * | 2022-03-16 | 2022-06-07 | 浙江大学 | Preparation method and application of pyridazine-doped modified C3N4 photocatalyst |
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