CN107349901A - A kind of mesoporous nitridation carbon adsorbing material and its preparation method and application - Google Patents
A kind of mesoporous nitridation carbon adsorbing material and its preparation method and application Download PDFInfo
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- CN107349901A CN107349901A CN201710662399.3A CN201710662399A CN107349901A CN 107349901 A CN107349901 A CN 107349901A CN 201710662399 A CN201710662399 A CN 201710662399A CN 107349901 A CN107349901 A CN 107349901A
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- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
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- 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
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- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C01P2006/16—Pore diameter
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- 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
- C02F2101/34—Organic compounds containing oxygen
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- 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
- C02F2101/36—Organic compounds containing halogen
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- 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
- C02F2101/38—Organic compounds containing nitrogen
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Abstract
The present invention discloses a kind of mesoporous nitridation carbon adsorbing material and its preparation method and application.This method is that cyanamide is added in silicon dioxide gel, it is heated to being dried in vacuo after being thoroughly mixed, it will be calcined after gained solid abrasive at 450~550 DEG C, calcined product is added in ammonium hydrogen fluoride solution, stirring, filter, wash and be dried in vacuo, after it is cooled to room temperature, grinding, sieving, obtains mesoporous nitridation carbon adsorbing material.This method uses simple thermal polymerization, and materials synthesis technique is simple, reproducible, can be mass produced.The mesoporous carbonitride of gained (mpg C3N4) there is very high specific surface area, effective antibiotic adsorbent can be used as, its adsorption process is simple to operation, energy consumption is low, adsorbance is high, can be used widely in field of antibiotics of degrading, and has higher application prospect and use value.
Description
Technical field
The invention belongs to absorbent fields, more particularly, to a kind of mesoporous nitridation carbon adsorbing material and preparation method thereof
And application.
Background technology
At present, antibiotic (such as Ofloxacin, Norfloxacin, Ciprofloxacin) has been widely used in medical treatment, animals and plants
Prevention and control of plant diseases, pest control etc..But after most antibiotics are absorbed by organisms, largely body can be discharged with excrement with parent fo
Outside, into environment.Into environment antibiotic can not only be killed under extremely low ambient concentration many floras in environment but also
The generation of anti-medicine flora is can induce, serious harm is caused to human health and the whole ecosystem.Therefore, it is a kind of to need development badly
The water technology of notable removal effect is known as to antibiosis in water environment.
The processing method of antibiotic waste water mainly has chemical oxidization method, microorganism treatment, photodissociation method and absorption method etc..Its
In, absorption method is easy to operate due to the advantages of its own such as energy consumption is small, should without adding that complicated dosing process etc. is easy to spread
With, and be particularly suitable for being used as advanced treatment process, for removing the pollutant removed in water body with conventional treatment process hardly possible, by
Increasing concern.Therefore, the research emphasis for being selected to absorption method of sorbing material.
Conventional adsorbent is broadly divided into natural adsorbent and synthetic adsorbent.But prepared by the adsorbent being currently known
Complex process, it is unfavorable for putting into production.Carbonitride (g-C3N4) it is a kind of new nonmetallic materials, it has stability high, malicious
Property is low, the advantages that easily preparing, and turns into a kind of new adsorbent.But because its low surface area causes its absorption to antibiotic to be imitated
Fruit is poor.
The content of the invention
In order to solve above-mentioned the shortcomings of the prior art, there is provided a kind of preparation of mesoporous nitridation carbon adsorbing material
Method.This method can obtain the sorbing material with high-specific surface area by this method, prepare simply, and can be with efficient absorption water
Middle testing afloqualone antibiotic.
Another object of the present invention is to provide the mesoporous nitridation carbon adsorbing material of above method preparation.
It is still another object of the present invention to provide the application of above-mentioned mesoporous nitridation carbon adsorbing material.
The purpose of the present invention is realized by following technical proposals：
A kind of preparation method of mesoporous nitridation carbon adsorbing material, is comprised the following specific steps that：
S1. cyanamide is added in silicon dioxide gel, is heated to being dried in vacuo after being thoroughly mixed, obtains solid A；
S2. in 450~550 DEG C of calcinings after solid A is ground, solid B is obtained；
S3. solid B is added in ammonium hydrogen fluoride solution, stirring, filters, washs and be dried in vacuo, treat that it is cooled to room
Wen Hou, grind, sieving, obtain mesoporous carbonitride (mpg-C3N4) sorbing material.
Preferably, the volume ratio of cyanamide and silicon dioxide gel described in step S1 is (5~8)：(3~6).
Preferably, the temperature heated described in step S1 is 50~70 DEG C, and the vacuum drying temperature is 50~70 DEG C,
The vacuum drying time is 18~24h.
Preferably, the time calcined described in step S2 is 3~4h, and the programming rate of the calcining is 2~3 DEG C/min.
Preferably, the concentration of ammonium acid fluoride described in step S3 is 4~6mol/L, and the time of the stirring is 48~72h,
The solution of the washing is ultra-pure water and absolute ethyl alcohol, and the temperature of the drying is 50~70 DEG C, and the time of the drying is 18
~24h.
Preferably, the mass volume ratio of solid B and ammonium hydrogen fluoride solution described in step S3 is (3-5)：(50-80)g/
mL。
A kind of mesoporous nitridation carbon adsorbing material is prepared by the above method.
Application of the mesoporous nitridation carbon adsorbing material in antibiotic of degrading.
Preferably, the antibiotic is testing afloqualone antibiotic.
It is further preferable that the testing afloqualone antibiotic is Ofloxacin, Norfloxacin, Ciprofloxacin, and Enrofloxacin, Lip river
One or more of U.S. husky star or fleraxacin.
Above-mentioned mesoporous adsorbent is as follows to the method for the absorption of antibiotic in water body：0.025g mesoporous adsorbents are weighed to be placed in
In beaker, 50mL4mg/L antibiotic solution is added.Adsorbed under agitation after ultrasonic 5min, use liquid chromatogram
Measure the amount of remaining antibiotic in solution.
Compared with prior art, the invention has the advantages that：
1. the mesoporous carbonitride (mpg-C of the present invention3N4) there is very high specific surface area, effective antibiotic can be used as
Adsorbent, its adsorption process is simple to operation, energy consumption is low, adsorbance is high.
2. the mpg-C of the present invention3N4Preparation method, using simple thermal polymerization, materials synthesis technique is simple, repeatability
It is good, there is the primary condition of large-scale production, there is higher application prospect and use value.
3. the present invention prepares the carbonitride (mpg-C with meso-hole structure by the Morphological control to carbonitride3N4), increase
Its big specific surface area is to improve the absorption to antibiotic in water body.
Brief description of the drawings
Fig. 1 is the mpg-C in embodiment 13N4With the g-C in comparative example 13N4TEM photos.
Fig. 2 is the mpg-C in embodiment 13N4With the g-C in comparative example 13N4Specific surface area.
Specific embodiment
Present disclosure is further illustrated with reference to specific embodiment, but should not be construed as limiting the invention.
Unless otherwise specified, the conventional meanses that technological means used in embodiment is well known to those skilled in the art.Except non-specifically
Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagent, method and apparatus.
Embodiment 1
A kind of preparation method of mesoporous nitridation carbon adsorbing material, comprises the following steps：
1. weighing 5mL cyanamides to be placed in alumina crucible, 3mL silica (SiO is added thereto2) colloidal sol, 50 DEG C
Heating water bath and stir 50 DEG C of dry 24h in vacuum drying chamber are placed in after being thoroughly mixed, obtain blocks of solid A.
2. transferred to after gained blocks of solid A is milled in Muffle furnace and rise to 550 DEG C with 3 DEG C/min programming rate,
And temperature 3h is kept, obtain faint yellow solid B.
3. gained faint yellow solid B3g is put into 50mL4mol/L ammonium acid fluoride, stirring 72h removes silica mould
Plate.Filtered afterwards and 50 DEG C of dry 24h in vacuum drying chamber are placed in after being washed with ultra-pure water and absolute ethyl alcohol, treat its cooling
To room temperature, mill, sieve, obtain mpg-C3N4- 1 adsorbent.
Comparative example 1
A kind of g-C3N4The preparation of adsorbent, comprises the following steps：
Weigh 5mL cyanamides to be placed in alumina crucible, be placed in 50 DEG C of baking ovens and dry 24h, after being cooled to room temperature, grind
Mill, sieving, obtains g-C3N4Adsorbent.
Fig. 1 is the mpg-C in embodiment 13N4With the g-C in comparative example 13N4TEM figure.Wherein (a) is g-C3N4、(b)
For mpg-C3N4.As shown in Figure 1, mpg-C3N4With obvious meso-hole structure, its diameter is about 12nm, and g-C3N4Presentation layer
Shape structure.
Fig. 2 is the mpg-C in embodiment 13N4With the g-C in comparative example 13N4Specific surface area.As shown in Figure 2, mpg-
C3N4Specific surface area be 141.271m2/ g, hence it is evident that more than body shape g-C3N4(16.746m2/g).According to Brunauer-Deming-
Teller (BDDT) classifies, mpg-C3N4N2Adsorption-desorption isothermal belongs to typical IV types, shows mpg-C3N4With typical case
Meso-hole structure.In addition, mpg-C3N4Pore-size distribution be concentrated mainly on 12nm or so, this result in TEM photos with being observed
Pore size it is consistent.As a result mpg-C is illustrated3N4With higher specific surface area, so as to provide more adsorption sites, carry
High adsorption efficiency.
Embodiment 2
A kind of preparation of mesoporous carbon nitride adsorbent, comprises the following steps：
1. weighing 5mL cyanamides to be placed in alumina crucible, 6mL silicon dioxide gels are added thereto, and 50 DEG C of water-baths add
Hot and stirring is placed in 50 DEG C of dry 24h in vacuum drying chamber to after being thoroughly mixed, and obtains blocks of solid A.
2. transferred to after gained blocks of solid A is milled in Muffle furnace and rise to 550 DEG C with 3 DEG C/min programming rate,
And temperature 3h is kept, obtain faint yellow solid B.
3. gained faint yellow solid B3g is put into 50mL4mol/L ammonium acid fluoride, stirring 72h removes silica mould
Plate.Filtered afterwards and 50 DEG C of dry 24h in vacuum drying chamber are placed in after being washed with ultra-pure water and absolute ethyl alcohol, treat its cooling
To room temperature, mill, sieve, obtain mpg-C3N4- 2 adsorbents.
Embodiment 3
1. weighing 8mL cyanamides to be placed in alumina crucible, 6mL silicon dioxide gels are added thereto, and 70 DEG C of water-baths add
Hot and stirring is placed in 70 DEG C of dry 18h in vacuum drying chamber to after being thoroughly mixed, and obtains blocks of solid A.
2. transferred to after gained blocks of solid A is milled in Muffle furnace and rise to 450 DEG C with 2 DEG C/min programming rate,
And temperature 4h is kept, obtain faint yellow solid B.
3. gained faint yellow solid B5g is put into 80mL6mol/L ammonium acid fluoride, stirring 48h removes silica mould
Plate.Filtered afterwards and 70 DEG C of dry 18h in vacuum drying chamber are placed in after being washed with ultra-pure water and sewage ethanol, treat its cooling
To room temperature, mill, sieve, obtain mpg-C3N4- 3 adsorbents.
Embodiment 4
Application of the mesoporous carbon nitride adsorbent of the present invention in antibiotic waste water processing, comprises the following steps：
1. obtained mpg-C in 25mg embodiments 1-3 is weighed respectively3N4-1、mpg-C3N4- 2 and mpg-C3N4- 3 adsorbents
In beaker, the Ofloxacin solution that 50mL concentration is 4mg/L is added, is positioned on six agitators, setting temperature is normal temperature.
2. the concentration C of liquid chromatogram measuring solution residue Ofloxacin is used after adsorbing 30min.According to formula N=(C0-
C) the clearance N, wherein C of * 100% calculating Ofloxacin0For the initial concentration of Ofloxacin.
3. weigh obtained g-C in 25mg comparative examples 13N4, repeat step 1 and step 2, it is husky to oxygen fluorine to obtain the adsorbent
The clearance of star.
Table 1 is adsorption efficiency of the different adsorbents to Ofloxacin in embodiment 1.As shown in Table 1, in same time
Under, mpg-C3N4Absorption to Ofloxacin is far above g-C3N4, for different mesoporous carbon nitride materials, mpg-C3N4- 1 is small
In mpg-C3N4The adsorbance of -2 pairs of Ofloxacins, this is probably caused by the reduction of meso-hole structure.
Adsorption rate of the 1 different adsorbents of table to Ofloxacin
| Carbon nitride adsorbent | Clearance (%) |
| mpg-C3N4-1 | 75.8% |
| mpg-C3N4-2 | 68.6% |
| mpg-C3N4-3 | 71.3% |
| g-C3N4 | 9.5% |
Embodiment 5
Application of the mesoporous carbon nitride adsorbent of the present invention in antibiotic waste water processing, comprises the following steps：
1. weighing 25mg implements mpg-C made from 13N4Adsorbent is placed in beaker, and it is 4mg/L to be separately added into 50ml concentration
Norfloxacin, Enrofloxacin, Ofloxacin, Ciprofloxacin, Lomefloxacin, Fleroxacin solution, be positioned over six agitators
On, setting temperature is normal temperature.
2. filtering out the catalyst remained in sample using syringe-driven filter after absorption 30min, and surveyed with liquid chromatogram
Determine the concentration C of solution residue antibiotic.According to formula N=(C0- C) the * 100% clearance N for calculating different antibiotic respectively, its
Middle C0For the initial concentration of antibiotic.
Table 2 is to implement clearance of 1 intermediary hole carbonitride to different antibiotic.As shown in Table 2, mpg-C3N4To promise
Flucloxacillin, Enrofloxacin, Ofloxacin, Ciprofloxacin, Lomefloxacin, the clearance of fleraxacin difference antibiotic 70% with
On, illustrate mpg-C3N4There is very strong adsorption effect.
Clearance of the 2 mesoporous carbonitride of table to different antibiotic
| Antibiotic | Clearance (%) |
| Ofloxacin | 75.8% |
| Enrofloxacin | 89.8% |
| Norfloxacin | 82.3% |
| Ciprofloxacin | 85.1% |
| Lomefloxacin | 70.2% |
| Fleraxacin | 73.5% |
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine and simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of mesoporous nitridation carbon adsorbing material, it is characterised in that comprise the following specific steps that：
S1. cyanamide is added in silicon dioxide gel, is heated to being dried in vacuo after being thoroughly mixed, obtains solid A；
S2. in 450~550 DEG C of calcinings after solid A is ground, solid B is obtained；
S3. solid B is added in ammonium hydrogen fluoride solution, stirring, filters, washs and be dried in vacuo, after it is cooled to room temperature,
Grinding, sieving, obtains mesoporous nitridation carbon adsorbing material.
2. the preparation method of mesoporous nitridation carbon adsorbing material according to claim 1, it is characterised in that described in step S1
The volume ratio of cyanamide and silicon dioxide gel is (5~8)：(3~6).
3. the preparation method of mesoporous nitridation carbon adsorbing material according to claim 1, it is characterised in that described in step S1
The temperature of heating be 50~70 DEG C, the vacuum drying temperature be 50~70 DEG C, the vacuum drying time be 18~
24h。
4. the preparation method of mesoporous nitridation carbon adsorbing material according to claim 1, it is characterised in that described in step S2
The time of calcining is 3~4h, and the programming rate of the calcining is 2~3 DEG C/min.
5. the preparation method of mesoporous nitridation carbon adsorbing material according to claim 1, it is characterised in that described in step S3
The concentration of ammonium acid fluoride is 4~6mol/L, and the time of the stirring is 48~72h, and the solution of the washing is ultra-pure water and nothing
Water-ethanol, the temperature of the drying is 50~70 DEG C, and the time of the drying is 18~24h.
6. the preparation method of mesoporous nitridation carbon adsorbing material according to claim 1, it is characterised in that described in step S3
The mass volume ratio of solid B and ammonium hydrogen fluoride solution is (3-5)：(50-80)g/mL.
7. a kind of mesoporous nitridation carbon adsorbing material, it is characterised in that the mesoporous nitridation carbon adsorbing material is by claim 1
Any one of~6 methods describeds are prepared.
8. application of the mesoporous nitridation carbon adsorbing material in antibiotic of degrading described in claim 7.
9. application of the mesoporous nitridation carbon adsorbing material in antibiotic of degrading according to claim 8, it is characterised in that described
Antibiotic is testing afloqualone antibiotic.
10. application of the mesoporous nitridation carbon adsorbing material in antibiotic of degrading according to claim 9, it is characterised in that institute
Testing afloqualone antibiotic is stated as Ofloxacin, Norfloxacin, Ciprofloxacin, Enrofloxacin, in Lomefloxacin or fleraxacin
More than one.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108686692A (en) * | 2018-03-30 | 2018-10-23 | 广东工业大学 | A kind of photochemical catalyst and its preparation method and application of oxygen doping carbonitride |
| CN109364974A (en) * | 2018-11-15 | 2019-02-22 | 江苏大学 | A kind of preparation method for the mesoporous azotized carbon nano material loading Pd-Co alloy |
| CN109384205A (en) * | 2018-09-21 | 2019-02-26 | 桂林理工大学 | A kind of superhard compound phase carbon nitride porous nano chain raw powder's production technology |
| CN110026229A (en) * | 2019-05-23 | 2019-07-19 | 重庆工商大学 | A kind of preparation method and applications of the mesoporous carbonitride of nitrogenous defect |
| CN110605136A (en) * | 2019-09-18 | 2019-12-24 | 宁夏大学 | Oxyfluorosaxing photocatalytic degradation material and preparation method thereof |
| CN111044586A (en) * | 2019-11-06 | 2020-04-21 | 江苏大学 | Preparation method of bismuth-doped polymeric carbon nitride nanocomposite material containing carbon defects |
| CN111153390A (en) * | 2020-01-19 | 2020-05-15 | 安徽大学 | Mesoporous graphite-phase carbon nitride material and preparation method and application thereof |
| CN111889122A (en) * | 2019-05-06 | 2020-11-06 | 天津大学 | Tungsten trioxide/graphite phase carbon nitride composite material and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108686692A (en) * | 2018-03-30 | 2018-10-23 | 广东工业大学 | A kind of photochemical catalyst and its preparation method and application of oxygen doping carbonitride |
| CN109384205A (en) * | 2018-09-21 | 2019-02-26 | 桂林理工大学 | A kind of superhard compound phase carbon nitride porous nano chain raw powder's production technology |
| CN109364974A (en) * | 2018-11-15 | 2019-02-22 | 江苏大学 | A kind of preparation method for the mesoporous azotized carbon nano material loading Pd-Co alloy |
| CN111889122A (en) * | 2019-05-06 | 2020-11-06 | 天津大学 | Tungsten trioxide/graphite phase carbon nitride composite material and preparation method thereof |
| CN111889122B (en) * | 2019-05-06 | 2021-07-27 | 天津大学 | Tungsten trioxide/graphite phase carbon nitride composite material and preparation method thereof |
| CN110026229A (en) * | 2019-05-23 | 2019-07-19 | 重庆工商大学 | A kind of preparation method and applications of the mesoporous carbonitride of nitrogenous defect |
| CN110605136A (en) * | 2019-09-18 | 2019-12-24 | 宁夏大学 | Oxyfluorosaxing photocatalytic degradation material and preparation method thereof |
| CN111044586A (en) * | 2019-11-06 | 2020-04-21 | 江苏大学 | Preparation method of bismuth-doped polymeric carbon nitride nanocomposite material containing carbon defects |
| CN111044586B (en) * | 2019-11-06 | 2022-03-22 | 江苏大学 | Preparation method of bismuth-doped polymeric carbon nitride nanocomposite material containing carbon defects |
| CN111153390A (en) * | 2020-01-19 | 2020-05-15 | 安徽大学 | Mesoporous graphite-phase carbon nitride material and preparation method and application thereof |
| CN111153390B (en) * | 2020-01-19 | 2022-04-08 | 安徽大学 | Mesoporous graphite-phase carbon nitride material and preparation method and application thereof |
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Application publication date: 20171117 |