CN108080016A - A kind of preparation method and application of potassium doping carbon nitride photocatalyst - Google Patents
A kind of preparation method and application of potassium doping carbon nitride photocatalyst Download PDFInfo
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- CN108080016A CN108080016A CN201711433773.9A CN201711433773A CN108080016A CN 108080016 A CN108080016 A CN 108080016A CN 201711433773 A CN201711433773 A CN 201711433773A CN 108080016 A CN108080016 A CN 108080016A
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- carbon nitride
- doping carbon
- potassium
- nitride photocatalyst
- potassium doping
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- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 23
- 239000011591 potassium Substances 0.000 title claims abstract description 23
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 23
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims abstract description 20
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 13
- 230000001699 photocatalysis Effects 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 235000010333 potassium nitrate Nutrition 0.000 claims abstract description 10
- 239000004323 potassium nitrate Substances 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- 230000015556 catabolic process Effects 0.000 claims abstract description 8
- 238000006731 degradation reaction Methods 0.000 claims abstract description 8
- 239000005416 organic matter Substances 0.000 claims abstract description 8
- 238000004321 preservation Methods 0.000 claims abstract description 8
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000007146 photocatalysis Methods 0.000 claims abstract description 4
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 3
- 238000010792 warming Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 10
- 238000012545 processing Methods 0.000 claims description 10
- 239000000975 dye Substances 0.000 claims description 5
- 238000005286 illumination Methods 0.000 claims description 5
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 4
- 229940012189 methyl orange Drugs 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 230000000630 rising effect Effects 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002052 molecular layer Substances 0.000 description 1
- IRPDISVJRAYFBI-UHFFFAOYSA-N nitric acid;potassium Chemical compound [K].O[N+]([O-])=O IRPDISVJRAYFBI-UHFFFAOYSA-N 0.000 description 1
- 239000001048 orange dye Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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—
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
A kind of preparation method and application of potassium doping carbon nitride photocatalyst.This method comprises the following steps:Ammonium chloride, dicyandiamide and potassium nitrate are mixed, when heat preservation 3~6 is small after being warming up to 500~600 DEG C;Cooled to room temperature after calcination, you can obtain above-mentioned potassium doping carbon nitride photocatalyst.The potassium doping carbon nitride photocatalyst is used for photocatalysis Decomposition organic matter.Photochemical catalyst produced by the present invention has larger interlamellar spacing and specific surface area, with excellent photocatalytic activity, in the degradation experiment to organic matter, its degradation efficiency is as many as twice of simple carbonitride, and simple possible, requirement to Experimental Establishment is relatively low, can utmostly save manufacturing cost.
Description
Technical field:
The present invention relates to a kind of potassium doping carbon nitride photocatalysts and its preparation method and application, belong to catalysis technique neck
Domain.
Background technology:
In recent years, with urbanization and the development of process of industrialization, the consumption of conventional fossil fuel increasingly increases, ground
The problem of ball energy storage amount drastically declines, energy shortage has caused the extensive concern of the mankind.In addition, it is fired by combusts fossil
The problem of environmental pollution that the processing of material and other trade wastes triggers also becomes increasingly conspicuous, and has seriously affected our daily life
It is living, threaten the sustainable development of human society.Based on this, seek a kind of environmentally protective, the reproducible energy is extremely urgent.
A kind of solar energy clean energy resource unlimited as reserves develops and utilizes the research hotspot as current researcher.
Photochemical catalyst can be under the irradiation of sunlight, under the excitation of photon, and electronics transits to conduction band by valence band and formed
Electron-hole pair degrades to organic pollution by a series of redox reaction.Entire reaction process only needs the sun
Illumination is the developing direction and trend of 21st century environmental pollution improvement without providing external energy.
Carbonitride can absorb visible ray (most light is accounted in sunlight), be because of its suitable energy gap
A kind of representative semiconductor light-catalyst.Yet with the short life of photo-generated carrier, the defects of recombination rate is high, limitation
The photocatalytic activity of carbonitride, it is therefore desirable to processing is modified to carbonitride to further improve reactivity.It is existing to grind
Study carefully and show that alkali-metal-doped processing is carried out to semiconductor light-catalyst can improve the conducting power of interface charge, inhibit photoproduction
Electron-hole pair it is compound, achieve the purpose that improve photocatalytic activity.
The content of the invention
The purpose of the present invention is for deficiency existing for current techniques, provide a kind of system of potassium doping carbon nitride photocatalyst
Preparation Method, this method add in potassium nitrate and ammonium chloride in the presoma of carbonitride, and the carbonitride light of directly obtained potassium doping is urged
Agent.Photochemical catalyst obtained has larger interlamellar spacing and specific surface area, has excellent photocatalytic activity, to organic matter
In degradation experiment, degradation efficiency is as many as twice of simple carbonitride.Simple possible of the present invention, requirement to Experimental Establishment compared with
It is low, manufacturing cost can be utmostly saved, there is very big development potentiality.
The technical scheme is that:
A kind of preparation method of potassium doping carbon nitride photocatalyst, includes the following steps:
(a) ammonium chloride and dicyandiamide are mixed, obtains the first mixture;Wherein, mass ratio is ammonium chloride:Dicyandiamide=
0.2~1:1;
(b) potassium nitrate with the first mixture obtained in step (a) is mixed again, obtains the second mixture;Wherein, quality
Than for potassium nitrate:Mixture=0.001~0.02 in step (a):1;
(c) the second mixture obtained in step (b) is placed in Muffle furnace or tube furnace and carried out in air at calcining
Reason, heating rate are 3~5 DEG C/min, when heat preservation 3~6 is small after being warming up to 500~600 DEG C;
(d) cooled to room temperature after calcination, you can above-mentioned potassium doping carbon nitride photocatalyst.
The application of the potassium doping carbon nitride photocatalyst, for photocatalysis Decomposition organic matter.
Comprise the following steps:The photochemical catalyst is added in into organic matter dye solution, is stirred under illumination or dark-state
When 1-3 is small, degradation is completed.
The organic matter dyestuff is preferably methyl orange.
Beneficial effects of the present invention are:
In the present invention, the carbon nitride photocatalyst that there is potassium to adulterate directly is prepared for by simple one-step method, simultaneously
The interlamellar spacing of carbonitride is made to become larger by adding in ammonium chloride, specific surface area dramatically increases, so as to add in light-catalyzed reaction
Active site achievees the purpose that improve photocatalytic activity.Under visible light illumination, the methyl of dyeing wastewater is simulated in experiment
Two hours degradation rates of orange solution just can reach more than 90%.
Description of the drawings
Fig. 1 is the sample pair prepared in Examples 1 to 3 in potassium doping carbon nitride photocatalyst and comparative example 1~2 obtained
Methyl orange dye reagent carries out the result of photocatalytic degradation.
Specific embodiment
Further illustrated the present invention below in conjunction with specific embodiments and the drawings, but embodiment the present invention is not done it is any
The restriction of form.Unless stated otherwise, the reagent of the invention used, method and apparatus is the art conventional reagent, methods
And equipment.
Unless stated otherwise, agents useful for same and material of the present invention are purchased in market.
Embodiment 1:
2g ammonium chlorides are taken, then the mixing of 10g dicyandiamides adds 0.05g potassium nitrate, is uniformly mixed, is subsequently placed in Muffle
Calcination processing is carried out in stove, heating rate is 5 DEG C/min, and when heat preservation 4 is small after rising to 550 DEG C, cooled to room temperature obtains institute
State potassium doping carbon nitride photocatalyst.
Embodiment 2:
5g ammonium chlorides are taken, 10g dicyandiamides and 0.1g potassium nitrate are uniformly mixed, are placed in Muffle furnace and carry out calcination processing, rise
Warm rate is 5 DEG C/min, and when heat preservation 4 is small after rising to 600 DEG C, cooled to room temperature obtains the potassium doping carbonitride light and urges
Agent.
Embodiment 3:
5g ammonium chlorides are taken, 10g dicyandiamides and 0.15g potassium nitrate are uniformly mixed, are placed in Muffle furnace and carry out calcination processing,
Heating rate is 3 DEG C/min, and when heat preservation 5 is small after rising to 550 DEG C, cooled to room temperature obtains the potassium doping carbonitride light
Catalyst.
Comparative example 1:
(parameter is identical with embodiment 1, and what is uniquely changed is to be not added with ammonium chloride and potassium nitrate) takes 10g dicyandiamides to be placed in
Calcination processing is carried out in Muffle furnace, heating rate is 5 DEG C/min, and when heat preservation 4 is small after rising to 550 DEG C, cooled to room temperature obtains
To simple carbon nitride photocatalyst.
Comparative example 2:
(parameter is identical with embodiment 1, and what is uniquely changed is to be not added with ammonium chloride) takes 10g dicyandiamides and 0.05g nitric acid
Potassium is uniformly mixed, and is placed in Muffle furnace and is carried out calcination processing, and heating rate is 5 DEG C/min, when heat preservation 4 is small after rising to 550 DEG C, from
It is so cooled to room temperature, obtains potassium doping carbon nitride photocatalyst.By measurement (N2 adsorption/desorption processing is carried out to sample, is utilized
Brunauer Emmett Teller, i.e. BET formula calculate the molecular layer volume of sample, so as to which specific surface be obtained, in of the invention
Use Kang Ta instrument companies of U.S. Quadrasorb SI automatic absorbings instrument) specific surface area of gained sample, in comparative example 1
The specific surface area of simple carbonitride is 18m2/ g, the specific surface area of sample is 23.6m in comparative example 22/ g, sample in embodiment 1
Specific surface is 79m2/g。
It can be seen that simple carbonitride (comparative example 1) under visible light has methyl orange the activity of photocatalytic degradation, right
There is (comparative example 2) photocatalytic activity after its progress potassium doping treatment is obviously improved, and ammonium chloride is added in preparation process into one
After step increase specific surface area (embodiment 1-3), photocatalytic activity reaches maximum, under visible light illumination, methyl orange solution
It can degrade to less than 5% within two hours.
The test condition of photocatalytic degradation is:Compound concentration is the methyl orange solution of 10mg/L, simulates dyeing wastewater.
After adding in 150mL dye solutions into photo catalysis reactor, the photochemical catalyst of 0.1g preparations is added, entire reaction process uses
Magnetic agitation persistently stirs.Dark reaction process is that reaction system is placed in darkroom, and absorption 30min ensures light-catalyzed reaction system
Reach adsorption equilibrium;Photocatalytic process is irradiated using xenon lamp simulated solar irradiation.Per 10min (dark reaction) or 20min, (light is urged
Change process) solution is taken to be detected, the absorbance of solution is measured after centrifugation in ultraviolet-visible spectrophotometer, is used for
Weigh its palliating degradation degree.
Unaccomplished matter of the present invention is known technology.
Claims (4)
1. a kind of preparation method of potassium doping carbon nitride photocatalyst, it is characterized in that this method comprises the following steps:
(a) ammonium chloride and dicyandiamide are mixed, obtains the first mixture;Wherein, mass ratio is ammonium chloride:Dicyandiamide=0.2~
1:1;
(b) potassium nitrate with the first mixture obtained in step (a) is mixed again, obtains the second mixture;Wherein, mass ratio is
Potassium nitrate:Mixture=0.001~0.02 in step (a):1;
(c) the second mixture obtained in step (b) is placed in Muffle furnace or tube furnace and carries out calcination processing in air, risen
Warm rate is 3~5 DEG C/min, when heat preservation 3~6 is small after being warming up to 500~600 DEG C;
(d) cooled to room temperature after calcination, you can above-mentioned potassium doping carbon nitride photocatalyst.
2. the application of potassium doping carbon nitride photocatalyst as described in claim 1, it is characterized in that organic for photocatalysis Decomposition
Object.
3. the application of potassium doping carbon nitride photocatalyst as claimed in claim 2, feature comprise the following steps:To organic matter
The photochemical catalyst is added in dye solution, when stirring 1-3 is small under illumination or dark-state, completes degradation.
4. the application of potassium doping carbon nitride photocatalyst as claimed in claim 2, feature include the organic matter dyestuff
For methyl orange.
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Cited By (14)
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CN108906099A (en) * | 2018-05-30 | 2018-11-30 | 常州科力尔环保科技有限公司 | Cu2S/g-C3N4The preparation method of heterojunction photocatalyst |
CN108927198A (en) * | 2018-07-09 | 2018-12-04 | 华南理工大学 | A kind of method that modified carbon nitride photocatalyst and its preparation synthesize xylonic with photochemical catalytic oxidation xylose |
CN108940338A (en) * | 2018-07-09 | 2018-12-07 | 湖南大学 | Potassium element adulterates nitride porous carbon photochemical catalyst and its preparation method and application |
CN109351362A (en) * | 2018-10-15 | 2019-02-19 | 广州中国科学院沈阳自动化研究所分所 | A kind of porous molecular doping carbon nitride photocatalyst and the preparation method and application thereof |
CN109395760A (en) * | 2018-11-16 | 2019-03-01 | 合肥能源研究院 | Catalysis oxidation furfural prepares catalyst of maleic acid and its preparation method and application |
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CN110560119A (en) * | 2019-08-14 | 2019-12-13 | 华东理工大学 | Preparation and application of potassium-doped inverse opal carbon nitride photocatalyst |
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CN105126893A (en) * | 2015-08-31 | 2015-12-09 | 中国科学院过程工程研究所 | Graphite-phase carbon nitride (g-C3N4) material and preparation method and application thereof |
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CN110240133A (en) * | 2019-07-03 | 2019-09-17 | 辽宁科技大学 | Potassium ion doped graphite phase carbon nitride nanosheet photocatalyst and preparation method thereof |
CN110240133B (en) * | 2019-07-03 | 2022-10-11 | 辽宁科技大学 | Potassium ion doped graphite phase carbon nitride nanosheet photocatalyst and preparation method thereof |
CN110560119A (en) * | 2019-08-14 | 2019-12-13 | 华东理工大学 | Preparation and application of potassium-doped inverse opal carbon nitride photocatalyst |
CN110449178A (en) * | 2019-09-05 | 2019-11-15 | 广州大学 | A kind of photochemical catalyst, preparation method and its application |
CN110449178B (en) * | 2019-09-05 | 2022-05-24 | 广州大学 | Photocatalyst, preparation method and application thereof |
CN111957345A (en) * | 2020-07-14 | 2020-11-20 | 广东工业大学 | 4-phenoxy phenol doped carbon nitride photocatalyst and preparation method and application thereof |
CN111957345B (en) * | 2020-07-14 | 2023-04-18 | 广东工业大学 | 4-phenoxy phenol doped carbon nitride photocatalyst and preparation method and application thereof |
CN112169750A (en) * | 2020-09-22 | 2021-01-05 | 北京化工大学 | Application of basic sylvite modified graphite-phase carbon nitride in preparation of cationic dye adsorbent |
CN113210005A (en) * | 2021-06-02 | 2021-08-06 | 成都理工大学 | Cl-doped C3N5And method for preparing the same |
CN113210005B (en) * | 2021-06-02 | 2022-07-26 | 成都理工大学 | Cl-doped C 3 N 5 And method for preparing the same |
CN113426470A (en) * | 2021-07-02 | 2021-09-24 | 中国科学技术大学 | Potassium, chlorine and iodine co-doped carbon nitride, preparation method thereof and method for preparing hydrogen peroxide through photocatalysis |
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