CN107456986A - The method that microwave quickly prepares mica load carbonitride catalysis material - Google Patents
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- 239000010445 mica Substances 0.000 title claims abstract description 85
- 229910052618 mica group Inorganic materials 0.000 title claims abstract description 85
- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 17
- -1 amine compound Chemical class 0.000 claims abstract description 17
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000011358 absorbing material Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 19
- 239000000725 suspension Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 10
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 239000004202 carbamide Substances 0.000 claims description 8
- 239000012774 insulation material Substances 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 238000005253 cladding Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- FAPDDOBMIUGHIN-UHFFFAOYSA-K antimony trichloride Chemical compound Cl[Sb](Cl)Cl FAPDDOBMIUGHIN-UHFFFAOYSA-K 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229920000877 Melamine resin Polymers 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000012670 alkaline solution Substances 0.000 claims description 4
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004964 aerogel Substances 0.000 claims description 2
- 239000003610 charcoal Substances 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 239000004965 Silica aerogel Substances 0.000 claims 1
- 150000001412 amines Chemical class 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- RJDOZRNNYVAULJ-UHFFFAOYSA-L [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] RJDOZRNNYVAULJ-UHFFFAOYSA-L 0.000 abstract 1
- 229910021383 artificial graphite Inorganic materials 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 229910001887 tin oxide Inorganic materials 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 description 16
- 238000006731 degradation reaction Methods 0.000 description 16
- 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 14
- 229940043267 rhodamine b Drugs 0.000 description 14
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 8
- 238000003756 stirring Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 229910002012 Aerosil® Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052571 earthenware Inorganic materials 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000007974 melamines Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
- 238000005406 washing Methods 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—
Abstract
The invention discloses a kind of method that microwave quickly prepares mica load carbonitride catalysis material, using two-dimensional sheet mica as carrier, one layer of microwave absorbing material tin oxide of Surface coating, material using amine compound as synthetic graphite carbonitride, mica load carbonitride catalysis material is prepared using microwave method.Tin ash has good Microwave Absorption Properties, is mixed with amine compound, the method combined by inside and outside microwave, expand the depth of microwave action, improve the efficiency and uniformity of microwave synthetic mica load carbonitride, shorten preparation time, greatly reduce the dosage of external microwave medium, economize on resources.
Description
Technical field
The present invention relates to a kind of method that microwave quickly prepares mica load carbonitride catalysis material.
Background technology
Photocatalytic self-cleaning technology is the photocatalysis based on inorganic semiconductor material, on the one hand degradable matrix surface
Organic pollution;On the other hand so that matrix surface is super hydrophilic, and matrix surface pollutant can fall with rain-out.Class graphite
Structure carbonitride (g-C3N4) it is a kind of semi-conducting material without metallic element, the Eg narrower (2.7eV) of the material, having can
See light absorpting ability, and its synthetic raw material is cheap, easily obtains, has great application prospect.In order to more preferably by g-
C3N4Apply based on cement on the external wall of material, by g-C3N4Cement base can effectively be prevented by being carried on mica sheet
Body neutral and alkali material is to g-C3N4Burn into embedding, so as to extend g-C3N4Service life.
The g-C of mica load at present3N4Based on mainly being synthesized with thermal polymerization, temperature is higher needed for this method, and required time
It is long, in a disguised form increase its production cost, hinder its industrial progress.Microwave method prepares carbonitride, and the time is short, energy consumption is small, raw
Produce efficiency high and technique is simple, be with a wide range of applications, but existing microwave prepares carbonitride method and will be mainly equipped with
Amine compound, as the container of urea is embedded in substantial amounts of microwave absorbing material, carbonitride is prepared by microwave heating, though this method
Preparation time so is shortened, but to consume substantial amounts of microwave absorbing material, causes the wasting of resources, and mica and amine compound are equal
Without Microwave Absorption Properties, can only be heated by external microwave absorbing medium by heat transfer, because microwave heating time is shorter,
So that can not fully it be heated inside the material of accumulation, so as to cause final products uniformity poor.
The content of the invention
It is an object of the invention to provide a kind of method that microwave quickly prepares mica load carbonitride catalysis material, make material
Material absorbs microwave in itself, so as to reduce extraneous microwave absorbing material dosage, while shortens the preparation time of carbonitride, improves product
Uniformity, its industrial production process is promoted, expands its application.
The technical scheme is that:The method that microwave quickly prepares mica load carbonitride catalysis material, its is specific
Step is as follows:
S1:Mica powder is placed in solvent, the weight/mass percentage composition of wherein mica powder accounts for 1%~20%, is stirred until homogeneous,
Ultrasonic disperse in ultrasonic wave is placed in, obtains two-dimentional mica sheet suspension;
S2:Mica sheet pH of suspension is adjusted to 1~2 with hydrochloric acid, 70~80 DEG C is heated to, adds a certain amount of SnCl4·
5H2O and SbCl3, wherein, SnCl4·5H2The mass ratio of O and mica is 0.5~2, SbCl3With SnCl4·5H2O mass ratioes are
0.05~0.2, mixing suspension pH value of solution is adjusted to 1~2 with alkaline solution, 2~4h is stirred, powder is centrifuged, wash, dried
It is dry, then powder is placed in high temperature furnace, is warming up to 600~800 DEG C, is incubated 2~3h, obtains the two of antimony-doped stannic oxide cladding
Tie up sheet mica;
S3:Two-dimentional mica and amine compound are uniformly mixed, wherein the mass ratio of two-dimentional mica and amine compound is
0.01~0.12:1;The crucible for being placed with two-dimentional mica and amine compound is placed in bigger crucible, inserted between two crucibles
Microwave absorbing material, in one layer of aeroge insulation material of crucible outer wrap, big crucible is put into microwave device, certain micro-
Under wave power, after heating a period of time, cooling obtains mica load carbonitride catalysis material.
The supersonic frequency of ultrasonic disperse in preferred steps S1 is 100W-500W, and ultrasonic time is 2~4h.
Solvent in preferred steps S1 is one or both of deionized water or ethanol mixed liquor.
Alkaline solution described in preferred steps S2 is sodium hydroxide solution or ammoniacal liquor.
Amine compound described in preferred steps S3 is the one or more in urea, melamine or dicyandiamide.
Aeroge insulation material described in preferred steps S3 is aerosil, fibrofelt aeroge or titanium dioxide
Silicon-fibrofelt composite aerogel.
Microwave power 350W-700W described in preferred steps S3.
Microwave time 10min-30min described in preferred steps S3.
Microwave absorbing material described in preferred steps S3 is unformed charcoal, CuO, Fe3O4、MnO2、SnO2Or WO3。
Beneficial effect:
Tin ash has good Microwave Absorption Properties, is mixed with amine compound, the side combined by inside and outside microwave
Method, expand the depth of microwave action, improve the efficiency and uniformity of microwave synthesis carbonitride, greatly reduce external microwave medium
Dosage, economize on resources.
Brief description of the drawings
Fig. 1 is that microwave heats the XRD that mica loads carbonitride catalysis material with obtaining two-dimentional mica after urea admixture
Figure;
Fig. 2 is that microwave heats mica with obtaining two-dimentional mica load carbonitride catalysis material degraded sieve after urea admixture
Red bright B performance maps, mica load carbonitride prepared by the technique have preferable rhodamine B degradation performance;
Fig. 3 is that microwave heats mica with obtaining two-dimentional mica load carbonitride catalysis material drop after melamine mixture
Rhodamine B performance map is solved, mica load carbonitride prepared by the technique has preferable rhodamine B degradation performance;
Fig. 4 is that microwave heats mica with obtaining two-dimentional mica load carbonitride catalysis material degraded after dicyandiamide mixture
Rhodamine B performance map, mica load carbonitride prepared by the technique have preferable rhodamine B degradation performance;
Fig. 5 is that microwave heats mica with obtaining two-dimentional mica load carbonitride catalysis material degraded sieve after urea admixture
Red bright B performance maps, mica load carbonitride prepared by the technique have preferable rhodamine B degradation performance.
Embodiment
Below in conjunction with the accompanying drawings with four embodiments, technical scheme is further introduced
Embodiment 1
Microwave described in the implementation case quickly prepares the preparation method of two-dimentional mica load class graphitic nitralloy carbon, including with
Lower step:
S1:5g mica powders are placed in 200mL ethanol, the weight/mass percentage composition of mica powder is 3%, is stirred until homogeneous, is placed in
In 400W ultrasonic waves, ultrasonic 2h, two-dimentional mica sheet suspension is obtained;
S2:Mica sheet pH of suspension is adjusted to 1.5 with hydrochloric acid, 70 DEG C is heated to, adds 5g SnCl4·5H2O and
1gSbCl3, mixed solution pH is adjusted to 1.5 with NaOH solution, stirs 3h, filters, wash, dry, powder is then placed in horse
Not in stove, 600 DEG C are warming up to, is incubated 3h, obtains the mica sheet of antimony-doped stannic oxide cladding;
S3:Weigh 0.2g two dimensions mica and 20g urea uniformly mixes;Mixture is placed in 100mL crucibles, by 100mL
Crucible is placed in 300mL crucibles, inserts a certain amount of CuO between two crucibles, and CuO piling height is equal to small crucible between two crucibles
The piling height of interior mixture, in one layer of fiber felt aeroge insulation material of 300mL crucibles outer wrap.By 300mL crucibles
It is placed in microwave device, the microwave 15min under 550w power, is cooled to room temperature and obtains two-dimentional mica load carbonitride photocatalysis material
Material.
As shown in Figure 1.By carrying out XRD tests to synthetic sample, analysis, which obtains synthetic sample, obvious g-C3N4, cloud
Female, SnO2Diffraction maximum.
Fig. 2 is that the mica prepared loads the rhodamine B degradation performance map of carbon nitride material, illustrates that prepared mica is born
Carrying carbon nitride material has the performance of preferable rhodamine B degradation, and 1 hour degradation rate is up to more than 95%.
Embodiment 2
S1:10g mica powders are placed in 100mL solvents, solvent is ethanol and deionized water mixture (ethanol:Deionization
Water=3:7), the weight/mass percentage composition of mica powder is about 10%, is stirred until homogeneous, and is placed in 100W ultrasonic waves, ultrasonic 4h, is obtained
Two-dimentional mica sheet suspension;
S2:Mica sheet pH of suspension is adjusted to 2.0 with hydrochloric acid, 75 DEG C is heated to, adds 20g SnCl4·5H2O and
2.4g SbCl3, stir to being completely dissolved, mixed solution pH be adjusted to 2.0 with ammoniacal liquor, stirs 3h, filters, wash, dry, so
Powder is placed in Muffle furnace afterwards, is warming up to 700 DEG C, is incubated 2h, obtains the mica sheet of antimony-doped stannic oxide cladding;
S3:Weigh 0.6g two dimensions mica and 20g melamines uniformly mix;Mixture is placed in 100mL crucibles, then will
This crucible is put into 300mL crucible, and a certain amount of Fe is inserted in two crucibles3O4, Fe between two crucibles3O4Piling height be equal to
The piling height of mixture in small crucible, in 300mL crucible outer wrap layer of silicon dioxide aeroge insulation materials.Will
300mL crucibles are placed in microwave device, under 550w power after microwave 15min, are cooled to room temperature and are obtained two-dimentional mica load nitrogen
Change carbon catalysis material.
Fig. 3 is that the mica prepared loads the rhodamine B degradation performance map of carbon nitride material, illustrates that prepared mica is born
Carrying carbon nitride material has the performance of preferable rhodamine B degradation, and 2 hours degradation rates are up to 98%.
Embodiment 3
S1:20g mica powders are placed in 100mL solvents, the weight/mass percentage composition of mica powder is that 20% solvent is deionization
Water, it is stirred until homogeneous, is placed in 500W ultrasonic waves, ultrasonic 3h, obtains two-dimentional mica sheet suspension;
S2:Mica sheet pH of suspension is adjusted to 1.0 with hydrochloric acid, 80 DEG C is heated to, adds 10g SnCl4·5H2O and
0.6g SbCl3, stir to being completely dissolved, mixed solution be progressively added dropwise in mica suspension, will be mixed with ammonia spirit molten
Liquid pH is adjusted to 1.0, stirs 4h, powder centrifugation, washing, dries, then powder is placed in Muffle furnace, be warming up to 800 DEG C, insulation
2h, obtain the mica sheet of antimony-doped stannic oxide cladding;
S3:Weigh 0.4g two dimensions mica and 20g dicyandiamides uniformly mix;Mixture is placed in 100mL crucibles, then by this
Crucible is put into 300mL crucible, inserts a certain amount of CuO in two crucibles, and CuO piling height is slightly above small earthenware between two crucibles
The piling height of mixture in crucible, in one layer of fiber felt/aerosil insulation material of 300mL crucibles outer wrap.
300mL crucibles are placed in microwave device, 350w microwaves 10min after microwave 15min, is cooled to room temperature and obtains under 550w power
Two-dimentional mica loads carbonitride catalysis material.
Fig. 4 is that the mica prepared loads the rhodamine B degradation performance map of carbon nitride material, illustrates that prepared mica is born
Carrying carbon nitride material has the performance of preferable rhodamine B degradation, and 2 hours degradation rates are up to 98%.
Embodiment 4
Microwave described in the implementation case quickly prepares the preparation method of two-dimentional mica load class graphitic nitralloy carbon, including with
Lower step:
S1:5g mica powders are placed in 200mL ethanol, the weight/mass percentage composition of mica powder is 3%, is stirred until homogeneous, is placed in
In 400W ultrasonic waves, ultrasonic 2h, two-dimentional mica sheet suspension is obtained;
S2:Mica sheet pH of suspension is adjusted to 1.5 with hydrochloric acid, 70 DEG C is heated to, adds a certain amount of 5g SnCl4·5H2O
With 1g SbCl3, mixed solution pH is adjusted to 1.5 with NaOH solution, stirs 2h, filters, wash, dry, be then placed in powder
In Muffle furnace, 600 DEG C are warming up to, is incubated 3h, obtains the mica sheet of antimony-doped stannic oxide cladding;
S3:Weigh 1.2g two dimensions mica and 10g urea uniformly mixes;Mixture is placed in 100mL crucibles, by 100mL
Crucible is placed in 300mL crucibles, inserts a certain amount of CuO between two crucibles, and CuO piling height is less than small crucible between two crucibles
The piling height of interior mixture, one layer of fiber felt/aerosil insulation material outside 300mL crucibles.By 300mL
Crucible is placed in microwave device, the microwave 10min under 700w power, is cooled to room temperature and is obtained two-dimentional mica load carbonitride light and urges
Change material.
Fig. 5 is that the mica prepared loads the rhodamine B degradation performance map of carbon nitride material, illustrates that prepared mica is born
Carrying carbon nitride material has the performance of preferable rhodamine B degradation, and 1 hour degradation rate is up to more than 60%.
Claims (9)
1. the method that microwave quickly prepares mica load carbonitride catalysis material, it is comprised the following steps that:
S1:Mica powder is placed in solvent, the weight/mass percentage composition of wherein mica powder accounts for 1%~20%, is stirred until homogeneous, and is placed in
Ultrasonic disperse in ultrasonic wave, obtain two-dimentional mica sheet suspension;
S2:Mica sheet pH of suspension is adjusted to 1~2 with hydrochloric acid, 70~80 DEG C is heated to, adds a certain amount of SnCl4·5H2O and
SbCl3, wherein, SnCl4·5H2The mass ratio of O and mica is 0.5~2, SbCl3With SnCl4·5H2O mass ratioes be 0.05~
0.2, mixing suspension pH value of solution is adjusted to 1~2 with alkaline solution, 2~4h is stirred, powder is centrifuged, wash, dried, then
Powder is placed in high temperature furnace, is warming up to 600~800 DEG C, is incubated 2~3h, obtains the two-dimensional sheet of antimony-doped stannic oxide cladding
Mica;
S3:Two-dimentional mica and amine compound are uniformly mixed, wherein the mass ratio of two-dimentional mica and amine compound is 0.01
~0.12:1;The crucible for being placed with two-dimentional mica and amine compound is placed in bigger crucible, microwave is inserted between two crucibles
Absorbing material, in one layer of aeroge insulation material of crucible outer wrap, big crucible is put into microwave device, in certain microwave work(
Under rate, after heating a period of time, cooling obtains mica load carbonitride catalysis material.
2. according to the method for claim 1, it is characterised in that the supersonic frequency of the ultrasonic disperse in step S1 is 100W-
500W, ultrasonic time are 2~4h.
3. according to the method for claim 1, it is characterised in that the solvent in step S1 is one in deionized water or ethanol
Kind or two kinds of mixed liquors.
4. according to the method for claim 1, it is characterised in that the alkaline solution described in step S2 is sodium hydroxide solution
Or ammoniacal liquor.
5. according to the method for claim 1, it is characterised in that the amine compound described in step S3 is urea, melamine
One or more in amine or dicyandiamide.
6. according to the method for claim 1, it is characterised in that the aeroge insulation material described in step S3 is titanium dioxide
Silica aerogel, fibrofelt aeroge or silicon dioxide fiber felt composite aerogel.
7. according to the method for claim 1, it is characterised in that the microwave power 350W-700W described in step S3.
8. according to the method for claim 1, it is characterised in that the microwave time 10min-30min described in step S3.
9. according to the method for claim 1, it is characterised in that microwave absorbing material described in step S3 is unformed charcoal,
CuO、Fe3O4、MnO2、SnO2Or WO3。
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WO2019015356A1 (en) * | 2017-07-18 | 2019-01-24 | 南京工业大学 | Method for rapidly preparing mica-supported carbon nitride photocatalytic material by means of microwaves |
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2008034510A2 (en) * | 2006-09-20 | 2008-03-27 | Merck Patent Gmbh | Photocatalytically active coating |
CN103285920A (en) * | 2013-05-27 | 2013-09-11 | 东华大学 | Three-dimensional fiber-based aerogel catalyst carrier and preparation method thereof |
CN104415786A (en) * | 2013-09-04 | 2015-03-18 | 安徽大学 | Method for quickly preparing quasi-graphite-structure carbon nitride material by adopting microwave heating |
CN105536844A (en) * | 2015-12-15 | 2016-05-04 | 南京工业大学 | Amorphous carbon composite carbon nitride photocatalysis material and preparation method thereof |
CN106268907A (en) * | 2016-08-15 | 2017-01-04 | 南京工业大学 | A kind of two dimension Conductive mica load carbonitride catalysis material and preparation method thereof |
CN106582768A (en) * | 2016-12-29 | 2017-04-26 | 南京工业大学 | Preparation method of two-dimensional and three-dimensional carrier reinforced carbon nitride photocatalytic material |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9735427B2 (en) * | 2015-02-12 | 2017-08-15 | Yang Zhang | Method of producing triazine-based graphitic carbon nitride films |
CN105772056A (en) * | 2016-04-28 | 2016-07-20 | 成都理工大学 | Preparation method and application of graphite-phase carbon nitride photocatalysis material |
CN107456986A (en) * | 2017-07-18 | 2017-12-12 | 南京工业大学 | The method that microwave quickly prepares mica load carbonitride catalysis material |
-
2017
- 2017-07-18 CN CN201710585266.0A patent/CN107456986A/en active Pending
-
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Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2008034510A2 (en) * | 2006-09-20 | 2008-03-27 | Merck Patent Gmbh | Photocatalytically active coating |
CN103285920A (en) * | 2013-05-27 | 2013-09-11 | 东华大学 | Three-dimensional fiber-based aerogel catalyst carrier and preparation method thereof |
CN104415786A (en) * | 2013-09-04 | 2015-03-18 | 安徽大学 | Method for quickly preparing quasi-graphite-structure carbon nitride material by adopting microwave heating |
CN105536844A (en) * | 2015-12-15 | 2016-05-04 | 南京工业大学 | Amorphous carbon composite carbon nitride photocatalysis material and preparation method thereof |
CN106268907A (en) * | 2016-08-15 | 2017-01-04 | 南京工业大学 | A kind of two dimension Conductive mica load carbonitride catalysis material and preparation method thereof |
CN106582768A (en) * | 2016-12-29 | 2017-04-26 | 南京工业大学 | Preparation method of two-dimensional and three-dimensional carrier reinforced carbon nitride photocatalytic material |
Non-Patent Citations (1)
Title |
---|
俞中平: ""不同形貌氧化锡纳米材料的制备、掺杂与光催化性能"", 《中国优秀硕士学位论文全文数据库•工程科技Ⅰ辑》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2019015356A1 (en) * | 2017-07-18 | 2019-01-24 | 南京工业大学 | Method for rapidly preparing mica-supported carbon nitride photocatalytic material by means of microwaves |
CN114100658A (en) * | 2021-11-23 | 2022-03-01 | 湖南农业大学 | Carbon nitride/tungsten trioxide/sulfur-doped antimony oxychloride double-Z-shaped composite photocatalyst and preparation method and application thereof |
CN114100658B (en) * | 2021-11-23 | 2023-09-12 | 湖南农业大学 | Carbon nitride/tungsten trioxide/sulfur doped antimony oxychloride double-Z-type composite photocatalyst, and preparation method and application thereof |
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