CN106185847A - A kind of low-density ultralight carbonitride raw powder's production technology with oriented growth - Google Patents
A kind of low-density ultralight carbonitride raw powder's production technology with oriented growth Download PDFInfo
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- CN106185847A CN106185847A CN201610512965.8A CN201610512965A CN106185847A CN 106185847 A CN106185847 A CN 106185847A CN 201610512965 A CN201610512965 A CN 201610512965A CN 106185847 A CN106185847 A CN 106185847A
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- oriented growth
- carbonitride
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- ultralight
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- 239000000843 powder Substances 0.000 title claims abstract description 22
- 238000005516 engineering process Methods 0.000 title claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000004202 carbamide Substances 0.000 claims abstract description 7
- 235000013877 carbamide Nutrition 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 238000003801 milling Methods 0.000 claims description 2
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 8
- 238000006731 degradation reaction Methods 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 6
- 239000000975 dye Substances 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 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 3
- 229940043267 rhodamine b Drugs 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 238000010671 solid-state reaction Methods 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 238000003541 multi-stage reaction Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910000161 silver phosphate Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000007704 wet chemistry method Methods 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
- 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—
Abstract
A kind of low-density ultralight carbonitride raw powder's production technology with oriented growth, calcines 0.5h 10h at 500 DEG C 600 DEG C, after calcining terminates, obtains the low-density ultralight carbonitride powder body with oriented growth after cooling after carbamide or tripolycyanamide being ground；The present invention is with carbamide and tripolycyanamide as raw material, through calcining, uses solid phase method one-step synthesis to go out azotized carbon nano material, and the method technology is simple, it is not necessary to complex device, and the response time is short, and product purity is high, and whole technological process is simple, it is easy to accomplish industrialized production.
Description
Technical field
The present invention relates to a kind of low-density ultralight carbonitride raw powder's production technology with oriented growth, belong to nanometer light
The preparation of catalyst and field of semiconductor materials.
Background technology
Carbonitride is a kind of excellent semiconductor light-catalyst, and unique electronic band structure makes it show the visible of excellence
Light photocatalysis performance, have inexpensive nontoxic, catalysis activity is high, oxidability strong, good chemical stability, be widely used in
The aspects such as the depollution of environment, photolysis water hydrogen, carbon dioxide energy, are a kind of important multi-functional N-shaped low energy gaps (2.7eV)
Quasiconductor.
The catalytic effect of carbon nitride photocatalyst and actual requirement have huge gap at present, and research worker is by compound
Or doping vario-property is to promote its photocatalysis effect.Such as Na Tian etc., carbonitride and cerium oxide are compounded to form heterogeneous nodule structure,
5h Degradation of Phenol rate reaches 55% [Tian N, Huang H, Liu C, et al.In situ co-under visible light illumination
pyrolysis fabrication of CeO2/g-C3N4n–n type heterojunction for synchronously
promoting photo-induced oxidation and reduction properties[J].J.mater.chem.a,
2015,3:17120-17129.].Up-to-date result of study shows, the surface texture that many catalysis materials expose is to photocatalysis
Reactivity has tremendous influence.Leaf JINHUA etc. find to expose the Ag of high surface energy crystal face3PO4Nanocrystalline in visible light catalytic fall
Solve in Organic substance reaction and have high activity [Y.Bi, S.Ouyang, N.Umezawa, J.Cao, J.Ye, Facet Effect of
Single-Crystalline Ag3PO4 Sub-microcrystals onPhotocatalytic Properties,
Journal of the American Chemical Society,133(2011)6490-6492.].Have so synthesizing
The carbonitride of particular crystal plane orientation is necessary.
At present, the method that synthesis carbon nitride photocatalyst is used has wet chemistry method and solid reaction process.Solid state chemistry is anti-
Should be mankind's chemical reactions of contacting the earliest and applying, and industrially be widely used.Solid state reaction has itself
Intrinsic shortcoming, but solid state reaction process does not use solvent, and productivity is high and technical process is simple；Synthesis environmental pollution is little, can
Avoid contaminated wastewater；Can be by controlling the conditions such as the proportioning of reactant, temperature, time, it is achieved stepwise reaction, obtain metasable state
Compound.
Summary of the invention
The invention discloses a kind of low-density ultralight carbonitride raw powder's production technology with oriented growth, preparation process
Simply, it is not necessary to complex device, low cost, prepared carbonitride morphology microstructure is good, has oriented growth feature, and density is low, weight
Amount is light, under sunlight, organic dyestuff can be carried out fast degradation.
For reaching above-mentioned purpose, the technical solution used in the present invention is:
A kind of low-density ultralight carbonitride raw powder's production technology with oriented growth, grinds carbamide or tripolycyanamide
After calcine after 0.5h-10h at 500 DEG C-600 DEG C, cooling, obtain the low-density ultralight carbonitride powder body with oriented growth.
Described milling time is 10min～60min.
The present invention is further improved by, and the raw material after grinding is put in crucible, and close crucible.
The present invention is further improved by, and the filler ratio of described crucible is 1/3～4/5.
The present invention is further improved by, and is warming up to 500 DEG C-600 DEG C with the programming rate of 5 DEG C/min-20 DEG C/min.
The present invention is further improved by, and described calcining is carried out in high temperature furnace, Muffle furnace or atmosphere furnace.
The present invention is further improved by, and described cooling uses air cooling.
Compared with prior art, the present invention has following useful technique effect: the present invention with carbamide or tripolycyanamide is
Raw material, through calcining, uses solid phase method one-step synthesis to go out azotized carbon nano material, and the method technology is simple, it is not necessary to complex device,
Response time is short, and product purity is high, and whole technological process is simple, it is easy to accomplish industrialized production.Through nitridation prepared by the present invention
Carbon nanomaterial, has oriented growth feature, for platelet morphology.Bigger specific surface area contributes in dyestuff degradation process
In, substrate is adsorbed in its surface, is that photo-generate electron-hole isoreactivity species directly react with dyestuff, improves its photocatalysis
Effect, shows the test of rhodamine B catalytic degradation: at sunlight 60min, the degradation rate of dyestuff i.e. be can reach 90% with
On, there is the photocatalysis effect of excellence.
Further, by controlling 5 DEG C/min-20 DEG C/min of programming rate, temperature retention time 0.5h-10h improves C3N4Powder
The pattern of body.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the embodiment of the present invention 2 gained sample；
Fig. 2 is the SEM figure of the embodiment of the present invention 2 gained sample；
Fig. 3 is the rhodamine B catalytic degradation figure under sunlight of the embodiment of the present invention 2 gained sample.
Detailed description of the invention
The present invention is described in detail with embodiment below in conjunction with the accompanying drawings.
Embodiment 1
1) carbamide is put into agate mortar and grinds 10min；
2) crucible poured into by the raw material after grinding, and is added a cover by crucible and puts in Muffle furnace, and places quality on crucible cover
More than the weight of 100g, keep the preferable air-tightness of crucible；Wherein, the filler ratio of crucible is 1/3；
3) it is warming up to calcining heat 500 DEG C with the programming rate of 5 DEG C/min, is incubated 4h, after calcining terminates, crucible is taken out
Carry out quick air cooling, obtain the low-density ultralight carbonitride powder body with oriented growth.
Embodiment 2
1) tripolycyanamide is put into agate mortar and grinds 10min；
2) crucible poured into by the raw material after grinding, and is added a cover by crucible and puts in Muffle furnace, and places quality on crucible cover
More than the weight of 100g, keep the preferable air-tightness of crucible；Wherein, the filler ratio of crucible is 3/4；
3) it is warming up to calcining heat 550 DEG C with the programming rate of 10 DEG C/min, is incubated 4h, after calcining terminates, crucible is taken
Go out to carry out quick air cooling, obtain the low-density ultralight carbonitride powder body with oriented growth.
From figure 1 it appears that prepared carbonitride has crystalline character, the growth of (002) high preferred orientation is substantially；
From figure 2 it can be seen that prepared carbonitride is flake；
From figure 3, it can be seen that rhodamine B is in cloudy, turbid phase under sunlight, powder body to dye adsorption relatively strong,
Sunlight 60min, i.e. can reach more than 90% to the degradation rate of dyestuff, has the photocatalysis effect of excellence.
Embodiment 3
1) carbamide is put into agate mortar and grinds 20min；
2) crucible poured into by the raw material after grinding, and is added a cover by crucible and puts in atmosphere furnace, and places quality on crucible cover
More than the weight of 100g, keep the preferable air-tightness of crucible；Wherein, the filler ratio of crucible is 3/4；
3) it is warming up to calcining heat 580 DEG C with the programming rate of 17 DEG C/min, is incubated 2h, after calcining terminates, crucible is taken
Go out to carry out quick air cooling, obtain the low-density ultralight carbonitride powder body with oriented growth.
Embodiment 4
1) tripolycyanamide is put into agate mortar and grinds 30min；
2) crucible poured into by the raw material after grinding, and is added a cover by crucible and puts in Muffle furnace, and places quality on crucible cover
More than the weight of 100g, keep the preferable air-tightness of crucible；Wherein, the filler ratio of crucible is 4/5；
3) it is warming up to calcining heat 550 DEG C with the programming rate of 15 DEG C/min, is incubated 4h, after calcining terminates, crucible is taken
Go out to carry out quick air cooling, obtain the low-density ultralight carbonitride powder body with oriented growth.
Claims (7)
1. a low-density ultralight carbonitride raw powder's production technology with oriented growth, it is characterised in that by carbamide or three
After poly cyanamid calcines 0.5h-10h bundle after grinding at 500 DEG C-600 DEG C, cooling, the low-density obtaining having oriented growth is ultralight
Carbonitride powder body.
A kind of low-density ultralight carbonitride raw powder's production technology with oriented growth the most according to claim 1, its
Being characterised by, described milling time is 10min～60min.
A kind of low-density ultralight carbonitride raw powder's production technology with oriented growth the most according to claim 1, its
Being characterised by, the raw material after grinding is put in crucible, and close crucible.
A kind of low-density ultralight carbonitride raw powder's production technology with oriented growth the most according to claim 3, its
Being characterised by, the filler ratio of described crucible is 1/3～4/5.
A kind of low-density ultralight carbonitride raw powder's production technology with oriented growth the most according to claim 1, its
It is characterised by, is warming up to 500 DEG C-600 DEG C with the programming rate of 5 DEG C/min-20 DEG C/min.
A kind of low-density ultralight carbonitride raw powder's production technology with oriented growth the most according to claim 1, its
Being characterised by, described calcining is carried out in high temperature furnace, Muffle furnace or atmosphere furnace.
A kind of low-density ultralight carbonitride raw powder's production technology with oriented growth the most according to claim 1, its
Being characterised by, described cooling uses air cooling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610512965.8A CN106185847A (en) | 2016-07-01 | 2016-07-01 | A kind of low-density ultralight carbonitride raw powder's production technology with oriented growth |
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| CN201610512965.8A CN106185847A (en) | 2016-07-01 | 2016-07-01 | A kind of low-density ultralight carbonitride raw powder's production technology with oriented growth |
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| CN106185847A true CN106185847A (en) | 2016-12-07 |
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| CN201610512965.8A Pending CN106185847A (en) | 2016-07-01 | 2016-07-01 | A kind of low-density ultralight carbonitride raw powder's production technology with oriented growth |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106622331A (en) * | 2017-01-06 | 2017-05-10 | 广西民族大学 | Preparation method of high-specific-surface-area graphite phase carbon nitride photocatalyst |
| CN107344714A (en) * | 2017-07-28 | 2017-11-14 | 西安理工大学 | A kind of preparation method of black g C3N4 powder |
| CN113238005A (en) * | 2021-05-12 | 2021-08-10 | 陕西科技大学 | N/CoTiO with alcohol-sensitive aldehyde-sensitive dual functions3@g-C3N4Composite material and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106622331A (en) * | 2017-01-06 | 2017-05-10 | 广西民族大学 | Preparation method of high-specific-surface-area graphite phase carbon nitride photocatalyst |
| CN106622331B (en) * | 2017-01-06 | 2019-06-14 | 广西民族大学 | A kind of preparation method of high-specific surface area graphite phase carbon nitride photochemical catalyst |
| CN107344714A (en) * | 2017-07-28 | 2017-11-14 | 西安理工大学 | A kind of preparation method of black g C3N4 powder |
| CN113238005A (en) * | 2021-05-12 | 2021-08-10 | 陕西科技大学 | N/CoTiO with alcohol-sensitive aldehyde-sensitive dual functions3@g-C3N4Composite material and preparation method and application thereof |
| CN113238005B (en) * | 2021-05-12 | 2024-01-23 | 深圳万知达科技有限公司 | N/CoTiO with alcohol-sensitive aldehyde-sensitive dual functions 3 @g-C 3 N 4 Composite material, preparation method and application thereof |
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