CN109876845A - M-g-C3N4The preparation method and application of/rGOA composite adsorption visible light catalytic material - Google Patents
M-g-C3N4The preparation method and application of/rGOA composite adsorption visible light catalytic material Download PDFInfo
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Abstract
The present invention provides a kind of M-g-C3N4The preparation method and application of/rGOA composite adsorption visible light catalytic material, it include: that melamine 1) is added in 80 DEG C~90 DEG C of deionized water, after being cooled to room temperature, hydrochloric acid is added and stirs, the molar ratio of melamine and hydrochloric acid is 1:0.5~1:2, and evaporation drying obtains melamine hydrochloride；Melamine hydrochloride is put into Muffle furnace, 500 DEG C and keeps 2h, then heats to 520 DEG C of holding 2h, cooling grinding obtains M-g-C3N4；2) by M-g-C3N4It is add to deionized water ultrasound；Graphene oxide is added；The sodium hydrogensulfite of certain mass is added in graphene oxide liquid mixture, ultrasound, heating obtain hydrogel, and hydrogel is then removed foreign ion and is freeze-dried.The composite material obtained using the method for the present invention effectively can be adsorbed and be degraded to organic dyestuff and antibiotic.
Description
Technical field
The present invention relates to environment and technical field of chemistry more particularly to a kind of M-g-C3N4/ rGOA composite adsorption visible light is urged
Change the preparation method and application of material.
Background technique
Organic dyestuff pollution is one of important sources of water environment pollution, with the fast development of world industry, especially
Developing country, the annual output of organic dyestuff is 7 × 105T is widely used in papermaking, leather processing, dope dyeing, makeup
The industries such as product and drug manufacture.China is antibiotics production and using big country, detected in environment water at present Ah
The Multiple Classes of Antibiotics such as Amdinocillin and Cefotaxime Sodium.The method for solving the problems, such as the organic contaminations such as dyestuff and antibiotic at present has biology
Degradation, physical and chemical adsorption, advanced oxidation and visible light catalytic etc..Since the method for visible light catalytic both can be energy saving,
Can degrade organic contamination again, so having obtained extensive concern.
Graphite phase carbon nitride (g-C3N4) it is used as a kind of non-metallic catalyst, adjustable band-gap width is 1.8~2.7eV, object
Physicochemical property is stablized, nontoxic, pollution-free, it is seen that optical response range is wide, under conditions of visible light there is good catalysis to live
Property.Graphite oxide aerogel (Graphene Oxide Aerogels, GOA) compares table as a kind of emerging carbon material with it
The feature that face is big, density is small, elastic high and absorption is strong, receives the concern of more and more researchers.Biggish specific surface area is not
Only attachment site can be provided for powder photocatalytic material also has good adsorption capacity, and in addition good electric conductivity can mention
The transmission efficiency of high electronics effectively inhibits the compound of electron-hole.There is easily recycling compared with two-dimensional graphene and reuse
The characteristics of.In addition, three-dimensional grapheme aeroge can also by control graphene oxide concentration and reactor shape come
Regulate and control shape, size and the density of aeroge.Therefore, needing one kind, to can be used for efficient absorption visible light photocatalytic degradation organic
Waste water, and can preferably be applied to the three-dimensional grapheme aerogel composite of Practical Project.
Summary of the invention
The present invention provides a kind of M-g-C3N4The preparation method and application of/rGOA composite adsorption visible light catalytic material, with
Solve problem above.
To achieve the goals above, this invention takes following technical solutions.
The present invention provides a kind of M-g-C3N4The preparation method of/rGOA composite adsorption visible light catalytic material, including it is as follows
Step:
(1)M-g-C3N4Preparation:
Melamine is added in 80 DEG C~90 DEG C of deionized water, after solution temperature is cooled to room temperature, to described molten
A certain amount of hydrochloric acid is added in liquid and constantly stirs, the molar ratio of melamine and hydrochloric acid is 1:0.5~1:2, is stirred evenly
Evaporation drying is carried out afterwards obtains melamine hydrochloride；The melamine hydrochloride is put into Muffle furnace, is heated to 500
DEG C and keep 2h, be then heated to 520 DEG C and keep 2h, finally cooling grinding obtains flaxen M-g-C3N4；
(2)M-g-C3N4The preparation of/rGOA:
By a certain amount of M-g-C3N4It is add to deionized water ultrasound and obtains M-g-C3N4Mixed liquor；To the M-
g-C3N4A certain amount of graphene oxide is added in mixed liquor and obtains graphene mixed liquor；It is added in the graphene mixed liquor
The sodium hydrogensulfite of certain mass, it is ultrasonic to uniformly mixed again；2.5~3.0h is heated at 95 DEG C using air dry oven,
The hydrogel is removed foreign ion by obtained hydrogel, freeze-drying obtains M-g-C3N4/ rGOA composite adsorption visible light
Catalysis material.
Preferably, the molar ratio of melamine and hydrochloric acid is 1:1.
Preferably, M-g-C3N4Mass ratio with graphene oxide is (2:9)~(6:9).
Preferably, M-g-C3N4Mass ratio with graphene oxide is 3:9
Preferably, the graphene oxide in step (2) is prepared using the Hummers method of modification.
Preferably, the additional amount of the sodium hydrogensulfite in step (2) is 6~7mg/mL.
Preferably, the evaporation drying in step (1) uses 80 DEG C of freeze-day with constant temperature of air dry oven.
Another aspect of the present invention, using M-g-C3N4The M- of the method preparation of/rGOA composite adsorption visible light catalytic material
g-C3N4/ rGOA composite adsorption visible light catalytic material, for the sewage treatment of organic dyestuff and antibiotic, to organic dyestuff and
Antibiotic carries out absorption and visible light photocatalytic degradation.
By the M-g-C of aforementioned present invention3N4The preparation method and application of/rGOA composite adsorption visible light catalytic material, can be with
Find out the M-g-C that method of the invention obtains3N4/ rGOA composite material is under conditions of radiation of visible light, M-g-C3N4It generates
Photoelectron can be quickly transferred on rGO lamella by a plurality of electron transfer pathways, effective to inhibit answering for electron-hole pair
It closes, gives full play to the catalytic performance of photochemical catalyst；Composite material of the invention is macroscopic three dimensional structure, is not only g-C3N4It provides
Attachment site, while adsorption site also is provided for pollutant, it is easily recycled.It is contaminated using composite degradation of the invention
Waste water catalytic efficiency with higher is expected, than simple M-g-C3N4It is more easily recycled recycling, is conducive to environment and the energy again
It utilizes；Mechanical resistance can be good, and cycle performance is excellent, simple production process.
The additional aspect of the present invention and advantage will be set forth in part in the description, these will become from the following description
Obviously, or practice through the invention is recognized.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this
For the those of ordinary skill of field, without creative efforts, it can also be obtained according to these attached drawings others
Attached drawing.
Fig. 1 is rGOA, M-g-C3N4、M-g-C3N4The SEM of/rGOA composite adsorption visible light catalytic material schemes, and (a, b) is
The SEM of rGOA schemes, and (c) is M-g-C3N4The SEM of/rGOA composite adsorption visible light catalytic material schemes, and (d) is M-g-C3N4SEM
Figure；
Fig. 2 is M-g-C3N4The x-ray diffraction map of/rGOA composite adsorption visible light catalytic material；
Fig. 3 is M-g-C3N4The BET of/rGOA composite adsorption visible light catalytic material schemes；
Fig. 4 is M-g-C3N4The absorption degradation tendency chart of/rGOA composite adsorption visible light catalytic material to antibiotic；
Fig. 5 is M-g-C3N4The absorption result figure of/rGOA composite adsorption visible light catalytic material to dyestuff；
Fig. 6 is M-g-C3N4The visible light catalytic result figure of/rGOA composite adsorption visible light catalytic material to dyestuff；
Fig. 7 is M-g-C3N4The circulation experiment result figure of/rGOA composite adsorption visible light catalytic material catalytic degradation dyestuff.
Specific embodiment
Embodiments of the present invention are described below in detail, the example of the embodiment is shown in the accompanying drawings, wherein from beginning
Same or similar element or element with the same or similar functions are indicated to same or similar label eventually.Below by ginseng
The embodiment for examining attached drawing description is exemplary, and for explaining only the invention, and is not construed as limiting the claims.
Those skilled in the art of the present technique are appreciated that unless expressly stated, singular " one " used herein, " one
It is a ", " described " and "the" may also comprise plural form.It is to be further understood that being arranged used in specification of the invention
Diction " comprising " refers to that there are the feature, integer, step and/or operations, but it is not excluded that in the presence of or addition it is one or more
Other features, integer, step, and/or the group of operation.It should be understood that wording "and/or" used herein includes one or more
A associated any cell for listing item and all combination.
Those skilled in the art of the present technique are appreciated that unless otherwise defined, all terms used herein (including technology art
Language and scientific term) there is meaning identical with the general understanding of those of ordinary skill in fields of the present invention.Should also
Understand, those terms such as defined in the general dictionary, which should be understood that, to be had and the meaning in the context of the prior art
The consistent meaning of justice, and unless defined as here, it will not be explained in an idealized or overly formal meaning.
In order to facilitate understanding of embodiments of the present invention, it is done by taking several specific embodiments as an example below in conjunction with attached drawing further
Explanation.
Embodiment
Present embodiments provide M-g-C3N4/ rGOA (mesoporous graphite phase carbon nitride/redox graphene aeroge) is compound
Adsorb the preparation method of visible light catalytic material, comprising the following steps:
Melamine is added to first in 80 DEG C~90 DEG C of deionized water, after solution temperature is cooled to room temperature,
37% hydrochloric acid (molar ratio of melamine and hydrochloric acid is 1:1) is added under magnetic agitation and constantly stirs, stirs 30min,
It is then placed in evaporation drying in 80 DEG C of air dry oven and obtains melamine hydrochloride；
Melamine hydrochloride is put into crucible with cover, with the heating rate of 20 DEG C/min in atmosphere formula Muffle furnace
It is heated to 500 DEG C and keeps 2h, be then heated to 520 DEG C with the heating rate of 4 DEG C/min and keep 2h；Cooling grinding obtains light
The M-g-C of yellow3N4。
By the M-g-C of obtained 60mg3N4It is add to deionized water ultrasonic 150min；Then graphene oxide is added
(Graphene Oxide, GO) is configured to the aqueous solution 60ml (M-g-C that GO concentration is 3.0mg/mL3N4With the matter of graphene oxide
Amount ratio is 3:9)；Weigh 512mg NaHSO3It is added in above-mentioned aqueous solution, ultrasonic 20min, is uniformly mixed；Ultrasound terminates
Afterwards, it moving it into air dry oven, heats 2.5h under 95 DEG C of environment, obtained hydrogel impregnates 6h using deionized water,
Period every 2h changes a water, and cleaning obtains the hydrogel of removal foreign ion；It is freeze-dried to obtain finally by freeze drier
M-g-C3N4/ rGOA composite adsorption visible light catalytic material.Fig. 1 is rGOA, M-g-C3N4、M-g-C3N4/ rGOA composite adsorption can
The SEM of light-exposed catalysis material schemes: Fig. 1 (a, b) is the SEM figure that rGOA amplifies different multiples, it can be seen that rGOA from figure (a)
(redox graphene aeroge) is made of two-dimentional rGO (redox graphene) lamellar structure, and figure (b) can be then more clear
Reaction pore structure, Fig. 1 (d) is it can be seen that M-g-C3N4Lamella block structure.RGOA layers of Fig. 1 (c) have squamous protrusion, illustrate two
Tie up sheet M-g-C3N4With rGOA adhesion.And it can be seen that corresponding layer structure and pore structure from Fig. 1 (c), so M-
The compound prototype structure without destroying rGOA of g-C3N4 and rGOA.
Fig. 2 is M-g-C3N4The x-ray diffraction map of/rGOA composite adsorption visible light catalytic material: referring to Fig. 2, M-g-
C3N4Mainly there are 13.1 ° and 27.2 ° two obvious diffraction maximums to occur, 13.1 ° of diffraction maximum corresponds to g-C3N4In structure
Period duplicate (100) crystal face in face, 27.2 ° of diffraction maximums correspond to conjugation interlayer and stack (002) crystal face.Crystal face (100) are deposited
Showing g-C3N4The plane of middle 5-triazine units connects.Single-phase rGOA is at 22.6 ° it can be observed that a wider diffraction maximum pair
That answer is loosely-packed (002) crystal face, M-g-C3N4M-g-C in/rGOA composite aerogel3N4Disappear in 13.1 ° of diffraction maximums
It loses, illustrates g-C3N4Crystal structure is changed in recombination process, this is because GO M-g-C in hydrothermal reaction process3N4
Thermal coupling effect, g-C have occurred between rGO3N427.2 ° of diffraction maximums can also be apparent observe, both illustrate at
Function is compound together.
Fig. 3 is M-g-C3N4The BET of/rGOA composite adsorption visible light catalytic material schemes: it can be seen that M-g- from Fig. 3 (a)
C3N4、rGOA、M-g-C3N4There is/rGOA composite adsorption visible light catalytic material biggish hysteresis loop to be belonged to according to IUPAC
IV type absorption-desorption thermoisopleth, caused by being the porous structure as present in sample.Therefore, three samples are in P/P0=0.45-
The characterization of adsorption of nitrogen is poor when 1.00, and hysteresis circulation shows to illustrate M-g-C there are hole3N4There are porositys.It can from Fig. 3 (b)
To find out, M-g-C3N4Aperture be mainly distributed at 2-50nm, in, macropore it is less.The aperture of rGOA is 2-5nm, M-g-
C3N4The aperture of/rGOA hydridization is 2-8nm, illustrates that the composite material of the embodiment of the present invention maintains original porous structure.
The M-g-C obtained using the embodiment of the present invention3N4/ rGOA composite adsorption visible light catalytic material is bearing to be more than certainly
Under 1600 times of pressure of body weight, still resilient, satisfactory mechanical property.
Simultaneously according to above-mentioned steps, the M-g-C of following mass ratio is prepared3N4/ rGOA composite adsorption visible light catalytic material:
M-g-C3N4: GO=6:9, M-g-C3N:GO=5:9, M-g-C3N4: GO=4:9, M-g-C3N4: GO=2:9, to carry out using real
It tests.
Application Example 1
Respectively by the M-g-C of 100mg3N4/ rGOA composite material (M-g-C3N4Mass ratio with graphene oxide is 3:
9) Amoxicillin (50mL, 2mg/L) and Cefotaxime Sodium antibiotic (50mL, 2mg/L) being distributed under magnetic stirring are water-soluble
In liquid, after dispersion, solution is placed under dark condition and adsorbs 30min.Then, it is placed in the 300W for filtering out 420nm or less wavelength
Xenon lamp radiation of visible light carries out antibiotic concentration analysis after 10min takes 3mL solution centrifugal filtration.All experiments repeat
Three times, guarantee the accuracy of experiment.Fig. 4 is absorption degradation tendency chart of the composite material to antibiotic.Referring to Fig. 4, rank is secretly adsorbed
Section, 30min is about 50% to the absorption of two kinds of antibiotic, it is seen that after light irradiates 60min, the removal of Cefotaxime Sodium (CFX)
Rate reaches 83.5%, and the removal rate of Amoxicillin (AMX) reaches 80%, shows that the composite material has good go to antibiotic
Except effect.
Application Example 2
The performance of sample by adsorbing rhodamine B in water and visible light degradation property is evaluated at room temperature.It will be preparatory
Above-mentioned different proportion (the M-g-C prepared3N4: GO=6:9, M-g-C3N:GO=5:9, M-g-C3N4: GO=4:9, M-g-
C3N4: GO=3:9, M-g-C3N4: GO=2:9) composite material, M-g-C3N4, rGOA respectively with rhodamine B solution (20mg/L,
It 100mL) is added in 250mL glass container, under dark condition, directly shows the absorption property of sample；Glass container is placed in
Under the 300W xenon lamp irradiation for filtering out 420nm or less wavelength, the absorption and light degradation ability of sample are showed.It is taken at interval of 20min
3mL solution, ultraviolet specrophotometer measure rhodamine B solution concentration at 551nm.Fig. 5 is M-g-C3N4/ rGOA composite adsorption
Absorption result figure of the visible light catalytic material to dyestuff；Fig. 6 is M-g-C3N4/ rGOA composite adsorption visible light catalytic material is to dye
The visible light catalytic result figure of material；Referring to Fig. 5, work as M-g-C3N4: GO is the M-g-C that 3:9 is obtained3N4/ rGOA composite material,
Under dark condition, 80min reaches 79% to Dye Adsorption removal rate；From fig. 6 it can be seen that under visible light illumination, 80min
Afterwards, M-g-C3N4: GO is that the M-g-C3N4/rGOA composite material absorption that 3:9 is obtained and visible light collaboration reach the removal rate of dyestuff
To 95%.
Using M-g-C3N4: GO is the M-g-C that 3:9 is obtained3N4It is taken after the completion of the adsorption experiment that/rGOA composite material carries out
After composite aerogel desorbs 1.5h in dehydrated alcohol out, 30min is impregnated with deionized water and removes dehydrated alcohol, is then dried again
Secondary reuse recycles above-mentioned photocatalysis experiment, the stability of test sample.Fig. 7 is M-g-C3N4/ rGOA composite adsorption is visible
The circulation experiment result figure of catalysis material catalytic degradation dyestuff, referring to Fig. 7, it can be seen that composite material of the invention uses
Processing cycle utilization, M-g-C are carried out afterwards3N4It is that 3:9 obtains M-g-C with rGOA3N4/ rGOA composite adsorption visible light catalytic material
Ring uses five results.The result shows that rhodamine B removal effect still reaches 90%, so sample has after being recycled five times
Good stability.
Those skilled in the art will be understood that above-mentioned application type is only for example, other are existing or are likely to occur from now on
Application type be such as applicable to the embodiment of the present invention, should also be included within the scope of protection of the present invention, and herein with reference side
Formula is incorporated herein.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with scope of protection of the claims
Subject to.
Claims (8)
1. a kind of M-g-C3N4The preparation method of/rGOA composite adsorption visible light catalytic material, which is characterized in that including walking as follows
It is rapid:
(1)M-g-C3N4Preparation:
Melamine is added in 80 DEG C~90 DEG C of deionized water, after solution temperature is cooled to room temperature, in Xiang Suoshu solution
A certain amount of hydrochloric acid is added and constantly stirs, the molar ratio of melamine and hydrochloric acid is 1:0.5~1:2, is stirred evenly laggard
Row evaporation drying obtains melamine hydrochloride；The melamine hydrochloride is put into Muffle furnace, is heated to 500 DEG C simultaneously
2h is kept, 520 DEG C is then heated to and keeps 2h, finally cooling grinding obtains flaxen M-g-C3N4；
(2)M-g-C3N4The preparation of/rGOA:
By a certain amount of M-g-C3N4It is add to deionized water ultrasound and obtains M-g-C3N4Mixed liquor；To the M-g-C3N4
A certain amount of graphene oxide is added in mixed liquor and obtains graphene mixed liquor；Certain matter is added in the graphene mixed liquor
The sodium hydrogensulfite of amount, it is ultrasonic to uniformly mixed again；2.5~3.0h is heated at 95 DEG C using air dry oven, is obtained
The hydrogel is removed foreign ion by hydrogel, freeze-drying obtains M-g-C3N4/ rGOA composite adsorption visible light catalytic material
Material.
2. preparation method according to claim 1, which is characterized in that the molar ratio of the melamine and hydrochloric acid is 1:
1。
3. preparation method according to claim 1, which is characterized in that the M-g-C3N4With the quality of graphene oxide
Ratio is (2:9)~(6:9).
4. preparation method according to claim 3, which is characterized in that the M-g-C3N4With the quality of graphene oxide
Ratio is 3:9.
5. preparation method according to claim 1, which is characterized in that the graphene oxide in the step (2) uses
It is prepared by the Hummers method of modification.
6. preparation method according to claim 1, which is characterized in that sodium hydrogensulfite in the step (2) plus
Entering amount is 6~7mg/mL.
7. preparation method according to claim 1, which is characterized in that the evaporation drying in the step (1) is using drum
80 DEG C of freeze-day with constant temperature of wind drying box.
8. M-g-C prepared by a kind of preparation method of any claim of claim 1-73N4/ rGOA composite adsorption visible light catalytic material
Material, which is characterized in that for the sewage treatment of organic dyestuff and antibiotic, absorption and visible is carried out to organic dyestuff and antibiotic
Photocatalytic degradation.
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| CN110624588A (en) * | 2019-09-23 | 2019-12-31 | 北京交通大学 | D-g-C3N4Preparation method and application of visible light catalytic material |
| CN111167496A (en) * | 2020-01-09 | 2020-05-19 | 南开大学 | Visible light catalytic material and preparation method and application thereof |
| CN111686688A (en) * | 2020-06-23 | 2020-09-22 | 广东工业大学 | Amino-modified graphene hydrogel and preparation method and application thereof |
| CN112919449A (en) * | 2021-02-08 | 2021-06-08 | 大连理工大学 | Boron-nitrogen co-doped porous carbon microsphere material and preparation method thereof |
| CN112973753A (en) * | 2021-03-01 | 2021-06-18 | 中国人民解放***箭军工程大学 | Preparation method and application of Z-type heterojunction aerogel type photocatalytic material |
| CN115772275A (en) * | 2022-11-30 | 2023-03-10 | 四川蓉仕环保科技有限公司 | Graphite-phase carbon nitride/nano-cellulose composite hydrogel, and preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110624588A (en) * | 2019-09-23 | 2019-12-31 | 北京交通大学 | D-g-C3N4Preparation method and application of visible light catalytic material |
| CN110624588B (en) * | 2019-09-23 | 2021-05-04 | 北京交通大学 | D-g-C3N4Preparation method and application of visible light catalytic material |
| CN111167496A (en) * | 2020-01-09 | 2020-05-19 | 南开大学 | Visible light catalytic material and preparation method and application thereof |
| CN111167496B (en) * | 2020-01-09 | 2020-12-25 | 南开大学 | Visible light catalytic material and preparation method and application thereof |
| CN111686688A (en) * | 2020-06-23 | 2020-09-22 | 广东工业大学 | Amino-modified graphene hydrogel and preparation method and application thereof |
| CN111686688B (en) * | 2020-06-23 | 2022-06-24 | 广东工业大学 | Amino-modified graphene hydrogel and preparation method and application thereof |
| CN112919449A (en) * | 2021-02-08 | 2021-06-08 | 大连理工大学 | Boron-nitrogen co-doped porous carbon microsphere material and preparation method thereof |
| CN112973753A (en) * | 2021-03-01 | 2021-06-18 | 中国人民解放***箭军工程大学 | Preparation method and application of Z-type heterojunction aerogel type photocatalytic material |
| CN115772275A (en) * | 2022-11-30 | 2023-03-10 | 四川蓉仕环保科技有限公司 | Graphite-phase carbon nitride/nano-cellulose composite hydrogel, and preparation method and application thereof |
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