CN109107589A - A kind of method and application preparing mesoporous sulfur modification ferroferric oxide/carbon nanotube complex - Google Patents
A kind of method and application preparing mesoporous sulfur modification ferroferric oxide/carbon nanotube complex Download PDFInfo
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- CN109107589A CN109107589A CN201811073672.XA CN201811073672A CN109107589A CN 109107589 A CN109107589 A CN 109107589A CN 201811073672 A CN201811073672 A CN 201811073672A CN 109107589 A CN109107589 A CN 109107589A
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- carbon nanotube
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
- C02F2101/345—Phenols
-
- 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
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
Abstract
The invention discloses a kind of method for preparing mesoporous sulfur modification ferroferric oxide/carbon nanotube complex and its applications in water process, include the following steps: for 0.1 g carbon nanotube to be dispersed in ultrasonic cell-break device in 50 ml deionized waters and handles 3 h, 0.02 mol ethanedioic acid is added to above-mentioned solution later, 50 DEG C are heated under magnetic agitation；By 5.56 g FeSO4·7H2O and 2.48 g Na2S2O3·5H2O mixed dissolution is added drop-wise in the above-mentioned solution containing carbon nanotube dropwise in 50 mL deionized waters, by mixed solution, forms yellow mercury oxide；Reactant is transferred in cryostat pot and cools to room temperature, suspended matter is filtered with vacuum filter, then 70 DEG C of dryings, and 300 DEG C of calcining 1h, heating rate are 4 DEG C of min to obtained yellow powder under nitrogen protection‑1；It is spare that final product is ground into powder.Catalyst prepared by the present invention has excellent catalytic properties, and realizes the removal of pollutant within a very short time, can adapt to broader pH model and good reusability, is expected to be used for the degradation of difficult removal pollutant.
Description
Technical field
The present invention relates to a kind of method for preparing mesoporous sulfur modification ferroferric oxide/carbon nanotube complex and its in Shui Chu
Application in reason belongs to the water treatment field in environmental protection.
Background technique
With the development of industry, in order to meet the growing material requisite of people, a large amount of waste water are generated in industrial production,
It relatively lags behind to the related research of these waste water removal, causes the worry of enterprise and society.Solve the problems, such as that this breach exists
In the strength by science, strengthens the prevention and improvement of water pollution, further increase the utilization rate of water resource.New period water pollution
Show complicated component, it is difficult the features such as, the requirement to minimizing technology is increasingly stringenter.Therefore, it is necessary to develop quick height
Effect, low in cost, the simple removal technology of operation and maintenance, to cope with this problem.
High-level oxidation technology (AOPs) is widely used in removing in pollutant, especially because of its impressive high efficiency
It is removal Recalcitrant chemicals.The one kind of Fenton technology as high-level oxidation technology, because its is easy to operate, reaction condition is mild,
The characteristics such as low in cost, environmental-friendly are widely used in removing in various pollutants.However, its narrow pH value working range,
Serious iron leaches the disadvantages of bring secondary pollution, restricts its widespread adoption.Class Fenton technology has been believed to
Effect improves these deficiencies of traditional Fenton, thus traditional Fenton technology is replaced to be widely used in degradation of contaminant.
In class Fenton technology, the preparation and selection of catalyst are particularly critical.There is ferroso-ferric oxide excellent magnetic to recycle
Property, it has received widespread attention.Research is many to the modified report of ferroso-ferric oxide, and the selection of carrier material is to catalytic among these
Can have a great impact.Carbon nanotube is special because of its high-specific surface area, excellent mechanical strength, hydrophobic surface and high electric conductivity
Levy deemed appropriate carrier material.In addition, catalysis caused by magnetic microsphere is reunited can be obviously improved after carbon material is modified
Activity inactivation.Recently, miscellaneous element is mixed to be believed to promote catalytic performance into catalyst.The doping of element sulphur has showed
It is improving the potentiality on catalytic performance out, this may be that the introducing of sulphur creates acidic micro-environment near catalyst, favorably
In the decomposition of hydrogen peroxide and the generation of hydroxyl radical free radical.
Therefore, mesoporous sulphur and the co-modified composite material of carbon nanotube are expected to realize that the collaboration of catalyst catalytic performance increases
By force, it is able to rapidly and efficiently degradation of contaminant.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for preparing mesoporous sulfur modification ferroferric oxide/carbon nanotube complex
And its application in water process is, it can be achieved that difficult for biological degradation in aquatic system within the scope of short period, wider PH
The efficient degradation of organic pollutant.
The present invention provides a kind of method for preparing mesoporous sulfur modification ferroferric oxide/carbon nanotube complex, including as follows
Step:
(1) it disperses 0.1 g carbon nanotube in 50 ml deionized waters, is ultrasonically treated 3 h with ultrasonic cell-break device, to
With.
(2) it takes 0.02 mol ethanedioic acid to be added to the dispersion liquid in step (1), and will be heated under mixture magnetic agitation
50 DEG C, for use.
(3) by 5.56 g FeSO4·7H2O and 2.48 g Na2S2O3·5H2O mixed dissolution in 50 ml deionized waters,
For use.
(4) dispersion liquid of step (2) will be added dropwise in step (3) containing ferrous solution, forms yellow mercury oxide.
(5) reactant is transferred to cryostat pot and cools to room temperature, suspended matter is filtered with vacuum filter, is then done for 70 DEG C
Dry, 300 DEG C of calcining 1h, heating rate are 4 DEG C of min to yellow powder under nitrogen protection-1。
(6) it is spare to be ground into powder for final catalyst.
Any one of carbon nanotube in multi-walled carbon nanotube, carboxylic carbon nano-tube used in step (1).
Ethanedioic acid used in step (2) be technical pure or it is analytically pure any one.
Dispersion liquid in step (2) is under magnetic agitation and 50 DEG C of atmosphere always before being put into cryostat pot.
FeSO in step (3)4·7H2O and Na2S2O3·5H2The molar ratio of O is 2:1.
The addition speed of strict control ferrous iron solution is answered in step (4).
The catalyst finally obtained in step (6) answers room temperature to be sealed.
This new catalyst of the method for the present invention preparation is characterized in that: carbon nanotube plays bracket work in the composite
With the effectively reunion of inhibition Fe 3 O 4 magnetic particle, so that these active microspheres are fully dispersed, while itself and pollutant
Strong bridging property can also be enriched with pollutant to its surface, and this modification helps to promote the mass transfer of pollutant.It is catalyzed after sulphur modification
Agent becomes solid acid medium, provides acidic micro-environment for pollutant catalysis, promotes the yield of hydroxyl radical free radical.
The present invention has the advantages that the carbon nanotube of bigger serface secures Fe 3 O 4 magnetic particle, prevent
The reunion of particle, and enrichment of the material to pollutant in water body is greatly strengthened, accelerate mass transfer of the pollutant to catalyst
Speed.The acidic micro-environment for being more advantageous to catalytic degradation is built in the modification of mesoporous sulphur, promotes free radical yield.It is prepared by the present invention
Catalyst has efficient catalytic performance, can adapt to broader PH range, and degradation rear catalyst is easy to divide from reaction system
From removal suitable for multiple pollutant.
Specific embodiment
To keep the above objects, features, and advantages of invention more obvious and easy to understand, below to specific implementation of the invention
Mode is described in detail.
Embodiment 1:
(1) it disperses 0.1 g carbon nanotube in 50 ml deionized waters, is ultrasonically treated 3 h with ultrasonic cell-break device, to
With.
(2) it takes 0.02 mol ethanedioic acid to be added to the dispersion liquid in step (1), and will be heated under mixture magnetic agitation
50 DEG C, for use.
(3) by 5.56 g FeSO4·7H2O and 2.48 g Na2S2O3·5H2O mixed dissolution in 50 ml deionized waters,
For use.
(4) dispersion liquid of step (2) will be added dropwise in step (3) containing ferrous solution, forms yellow mercury oxide.
(5) reactant is transferred to cryostat pot and cools to room temperature, suspended matter is filtered with vacuum filter, is then done for 70 DEG C
Dry, 300 DEG C of calcining 1h, heating rate are 4 DEG C of min to yellow powder under nitrogen protection-1。
(6) it is spare to be ground into powder for final catalyst.
The mesoporous sulfur modification ferroferric oxide/carbon nanotube complex of preparation is placed under transmission electron microscope (TEM)
The pattern of material is observed, in entire compound, a large amount of uniform ferroso-ferric oxide microballoons are attached to for discovery carbon nanotube crosslinking
Around carbon nanotube, without obvious agglomeration.Ferroferric oxide particle diameter is about 150-200 nm, carbon nanotube diameter
10-20 nm shows that the compound containing ferroferric oxide/carbon nanotube is synthesized.Catalyst is placed in neutral aqueous solution, is sent out
Existing solution ph is substantially reduced, it was demonstrated that sulphur is successfully modified on composite catalyst, and can build acidic micro-environment for reaction.
Embodiment 2:
(1) it disperses 0.1 g carbon nanotube in 50 ml deionized waters, is ultrasonically treated 3 h with ultrasonic cell-break device, to
With.
(2) it takes 0.02 mol ethanedioic acid to be added to the dispersion liquid in step (1), and will be heated under mixture magnetic agitation
50 DEG C, for use.
(3) by 5.56 g FeSO4·7H2O and 2.48 g Na2S2O3·5H2O mixed dissolution in 50 ml deionized waters,
For use.
(4) dispersion liquid of step (2) will be added dropwise in step (3) containing ferrous solution, forms yellow mercury oxide.
(5) reactant is transferred to cryostat pot and cools to room temperature, suspended matter is filtered with vacuum filter, is then done for 70 DEG C
Dry, 300 DEG C of calcining 1h, heating rate are 4 DEG C of min to yellow powder under nitrogen protection-1。
(6) it is spare to be ground into powder for final catalyst.
The catalyst of preparation is used to degrade the research of bisphenol-A (BPA), its catalytic performance is verified.10 mL 20 mg
L-1BPA solution be placed in 50 mL conical flasks, catalyst prepared by 2.0 mg will wherein be added.By being added 0.1 M's
H2SO4Or in the range of NaOH adjusting pH value of solution to 3.0-10.0.The H of known dose is added into system2O2It is anti-to cause Fenton
It answers.In entire reaction process, reaction solution is placed in shaking table with 250 r min-1Rate concussion, it is all test at room temperature
It carries out.In given time interval, 1.0 mL samples are collected, and 0.5 mL methanol quenching activity free radical are added immediately, so
Remaining solid particle is removed with the filtering of 0.22 micron membrane filter afterwards, the sample finally obtained be used to analyze the variation of BPA concentration.
By the variation of high performance liquid chromatography test b PA concentration, during finding PH from 3 to 10, in 15 min, the equal energy of removal rate
Reach close to 100%, shows that catalyst has wide pH working range, the degradation being adapted under the conditions of various pH.
Embodiment 3:
(1) it disperses 0.1 g carbon nanotube in 50 ml deionized waters, is ultrasonically treated 3 h with ultrasonic cell-break device, to
With.
(2) it takes 0.02 mol ethanedioic acid to be added to the dispersion liquid in step (1), and will be heated under mixture magnetic agitation
50 DEG C, for use.
(3) by 5.56 g FeSO4·7H2O and 2.48 g Na2S2O3·5H2O mixed dissolution in 50 ml deionized waters,
For use.
(4) dispersion liquid of step (2) will be added dropwise in step (3) containing ferrous solution, forms yellow mercury oxide.
(5) reactant is transferred to cryostat pot and cools to room temperature, suspended matter is filtered with vacuum filter, is then done for 70 DEG C
Dry, 300 DEG C of calcining 1h, heating rate are 4 DEG C of min to yellow powder under nitrogen protection-1。
(6) it is spare to be ground into powder for final catalyst.
Catalyst chooses the composite catalyst of ferroso-ferric oxide and above method preparation respectively, under the same conditions to implementation
BPA in example 2 carries out catalytic degradation, discovery ferroso-ferric oxide catalyst 15 min, or even longer time (4 h) almost without
BPA is removed, and composite catalyst can be achieved with completely removing in 15 min, it was demonstrated that this composite catalyst has excellent
Catalytic performance.
Embodiment 4:
(1) it disperses 0.1 g carbon nanotube in 50 ml deionized waters, is ultrasonically treated 3 h with ultrasonic cell-break device, to
With.
(2) it takes 0.02 mol ethanedioic acid to be added to the dispersion liquid in step (1), and will be heated under mixture magnetic agitation
50 DEG C, for use.
(3) by 5.56 g FeSO4·7H2O and 2.48 g Na2S2O3·5H2O mixed dissolution in 50 ml deionized waters,
For use.
(4) dispersion liquid of step (2) will be added dropwise in step (3) containing ferrous solution, forms yellow mercury oxide.
(5) reactant is transferred to cryostat pot and cools to room temperature, suspended matter is filtered with vacuum filter, is then done for 70 DEG C
Dry, 300 DEG C of calcining 1h, heating rate are 4 DEG C of min to yellow powder under nitrogen protection-1。
(6) it is spare to be ground into powder for final catalyst.
Three times by catalyst deionized water used in embodiment 2 and ethyl alcohol repeated flushing, it is dried in vacuo at 50 DEG C
Afterwards, it is re-used for degradation BPA, removal efficiency is still maintained at high level (96%) after finding 15 min, and it is good to show that catalyst has
Good reusability.
Claims (6)
1. a kind of method for the heterogeneous Fenton catalyst for preparing New Type of Mesoporous sulfur modification ferroferric oxide/carbon nanotube,
Be characterized in that method includes the following steps:
(1) it disperses 0.1 g carbon nanotube in 50 ml deionized waters, is ultrasonically treated 3 h with ultrasonic cell-break device, to
With；
(2) it takes 0.02 mol ethanedioic acid to be added to the dispersion liquid in step (1), and 50 will be heated under mixture magnetic agitation
DEG C, for use；
(3) by 5.56 g FeSO4·7H2O and 2.48 g Na2S2O3·5H2O mixed dissolution in 50 ml deionized waters, to
With；
(4) dispersion liquid of step (2) will be added dropwise in step (3) containing ferrous solution, forms yellow mercury oxide；
(5) reactant is transferred to cryostat pot and cools to room temperature, suspended matter is filtered with vacuum filter, then 70 DEG C of dryings, yellow
300 DEG C of calcining 1h, heating rate are 4 DEG C of min to color powder under nitrogen protection-1；
(6) it is spare to be ground into powder for final catalyst.
2. preparation method according to claim 1, which is characterized in that carbon nanotube used is selected from multi wall carbon in step (1)
Any one in nanotube, carboxylic carbon nano-tube.
3. preparation method according to claim 1, which is characterized in that cryostat pot is added in the mixed solution in step (2) certainly
It is constantly under magnetic agitation and 50 DEG C of atmosphere before.
4. preparation method according to claim 1, which is characterized in that FeSO used in step (3)4·7H2O and Na2S2O3·
5H2The molar ratio of O is 2:1.
5. preparation method according to claim 1, which is characterized in that be added dropwise in step (4) containing ferrous solution
The dispersion liquid of step (2).
6. preparation method according to claim 1, which is characterized in that the calcining of step (5) high temperature is under nitrogen protection,
Heating rate is 4 DEG C of min-1。
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Cited By (5)
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| CN109847764A (en) * | 2019-01-09 | 2019-06-07 | 哈尔滨工业大学 | A kind of methods and applications preparing sulphur modification ferriferous oxide film layer type Fenton catalyst |
| CN111013588A (en) * | 2019-12-16 | 2020-04-17 | 广东溢达纺织有限公司 | Fenton-like catalyst and preparation method and application thereof |
| CN112169727A (en) * | 2020-10-21 | 2021-01-05 | 哈尔滨理工大学 | Preparation method of halloysite-based micro-nano reactor for advanced catalytic oxidation |
| CN113659139A (en) * | 2021-07-12 | 2021-11-16 | 中北大学 | Vanadium sodium phosphate electrode material of vanadium-position copper-doped composite carbon nanotube and preparation method and application thereof |
| CN116037115A (en) * | 2023-01-29 | 2023-05-02 | 石河子大学 | Foam nickel-based CO-SCR denitration catalyst and preparation method thereof |
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| CN112169727B (en) * | 2020-10-21 | 2022-08-05 | 哈尔滨理工大学 | Preparation method of halloysite-based micro-nano reactor for advanced catalytic oxidation |
| CN113659139A (en) * | 2021-07-12 | 2021-11-16 | 中北大学 | Vanadium sodium phosphate electrode material of vanadium-position copper-doped composite carbon nanotube and preparation method and application thereof |
| CN116037115A (en) * | 2023-01-29 | 2023-05-02 | 石河子大学 | Foam nickel-based CO-SCR denitration catalyst and preparation method thereof |
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Application publication date: 20190101 |