CN110115975A - Modified carbon nitride adsorbent of a kind of manganese oxide and the preparation method and application thereof - Google Patents
Modified carbon nitride adsorbent of a kind of manganese oxide and the preparation method and application thereof Download PDFInfo
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- CN110115975A CN110115975A CN201910410814.5A CN201910410814A CN110115975A CN 110115975 A CN110115975 A CN 110115975A CN 201910410814 A CN201910410814 A CN 201910410814A CN 110115975 A CN110115975 A CN 110115975A
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- modified carbon
- carbon nitride
- manganese oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0259—Compounds of N, P, As, Sb, Bi
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/60—Heavy metals or heavy metal compounds
- B01D2257/602—Mercury or mercury compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
Abstract
The present invention provides modified carbon nitride adsorbents of a kind of manganese oxide and the preparation method and application thereof, the preparation method includes: that carbonitride is added in manganese nitrate solution, it is uniformly mixed and obtains suspension, it moves it in drying box and dries, then obtained solid is ground, gained powder is placed in again and burns boat and is subsequently moved in Muffle furnace and calcines, obtains the modified carbon nitride adsorbent of manganese oxide.The modified carbon nitride adsorbent of the manganese oxide that the present invention is prepared by simple incipient wetness at normal temperatures and pressures has large specific surface area, stability is strong, the characteristics of strong adsorption force, the Elemental Mercury in power-plant flue gas can effectively be removed, demercuration efficiency can achieve 95% under the high temperature conditions, and efficiency is apparently higher than traditional acticarbon.Adsorbent synthetic method of the present invention is simple, and material source is extensive, has good economy and industrial applicability, is a kind of Novel environment-friendlymaterial material.
Description
Technical field
The present invention relates to materialogy fields, and in particular to modified carbon nitride adsorbent of a kind of manganese oxide and preparation method thereof with
Using.
Background technique
Exploitation and utilization with the mankind to earth energy, bring industrial waste gas and waste water, have seriously polluted the environment, on
A lot of appalling severe events have occurred a century all over the world, such as Los Angeles,U.S city photochemical fog event, Japan
Minamata disease event and Fushan Mountain itai-itai event etc. finally compromise the health and personal safety of local resident.
It is waken up with a start just because of these severe event brings, people have gradually drawn lesson, start to pay attention to environment
Protection.In Japanese minamata disease event, heavy metal Hg causes serious baneful influence for the life of local several generations resident, draws
It plays scholar in world wide and starts the extensive concern to mercury.According to correlative study, the mercury emission of global coal-burning power plant accounts for the mankind
Various activities discharge the 65% of mercury total amount.Therefore, in recent years about coal-burning power plant's mercury pollution and its correlative study of emission control
It is increasingly becoming the research hotspot of countries in the world scholar.
Currently, flue active carbon spraying technique is to reduce coal-fired flue-gas mercury and mercuric compounds to discharge most general technology.But
Active carbon constrains its extensive industrial application due to adsorption capacity difference and economy etc., develops a kind of economical and efficient
Sorbent material become the task of top priority.
Summary of the invention
Invention is directed to the problems of the prior art, provides modified carbon nitride adsorbent of a kind of manganese oxide and preparation method thereof
It is poor to solve demercuration efficiency in the prior art with application, the technical problems such as operating cost height.
The present invention provides a kind of preparation methods of the modified carbon nitride adsorbent of manganese oxide characterized by comprising by nitrogen
Change carbon to be added in manganese nitrate solution, is uniformly mixed and obtains suspension, move it in drying box and dry, then by obtained solid
Grinding, then gained powder is calcined, obtain the modified carbon nitride adsorbent of manganese oxide.
Preferably, the carbonitride is made by melamine in the method for secondary clacining, specially first by melamine
It is placed in crucible in Muffle furnace and is warming up to 550 DEG C with the heating rate of 5 DEG C/min, calcine 2h, then set product grinding again
550 DEG C are warming up to the heating rate of 5 DEG C/min in Muffle furnace in calcining boat, calcines 2h to get carbonitride is arrived.
Preferably, the manganese nitrate solution is dissolved in deionized water by four water manganese nitrates and is prepared, the nitridation
The mass ratio of carbon and four water manganese nitrates is 0.15:0.023~0.049.
Preferably, the suspension drying temperature is 70 DEG C, and drying time is 6~8h.
Preferably, the calcining specifically: 2h is calcined to after 200 DEG C with the heating rate of 5 DEG C/min in Muffle furnace.
The present invention also provides the modified carbon nitride adsorbents of the manganese oxide of above method preparation.
The present invention also provides the modified carbon nitride adsorbents of the manganese oxide of above method preparation in flue gas demercuration adsorbent
Application.
Compared with prior art, the beneficial effects of the present invention are:
(1) the modified carbon nitride adsorbent of manganese oxide is prepared by straightforward procedure at normal temperatures and pressures the present invention provides a kind of
Method, use four water manganese nitrates, melamine as reactant, reaction dissolvent is deionized water, with incipient wetness system
Standby to obtain with large specific surface area, stability is strong, the new adsorbent of strong adsorption force.
(2) adsorbent prepared by the present invention can be used as the smoke evacuation such as coal-burning power plant, steel mill and garbage burning factory enterprise
Mercury removal adsorbent can effectively remove Elemental Mercury in flue gas by the way that adsorbent is placed in flue suitable position, in high temperature
Under the conditions of demercuration efficiency can achieve 95%, efficiency is apparently higher than traditional acticarbon, while the catalyst also can be used
In the adsorbing and removing of other pollutants.
(3) adsorbent prepared by the present invention has absorption property good, and stability is strong, and environmental pollution is small, preparation process letter
Single, the advantages that material source is extensive, technological progress is significant with conventional carbon spraying technique compared with, have good economy with
Industrial applicability.
Detailed description of the invention
Fig. 1 is the demercuration efficiency figure of embodiment 1 and embodiment 2 in the present invention；
Fig. 2 is the XRD diagram of embodiment 1 and embodiment 2 in the present invention；
Fig. 3 is the TEM figure of embodiment 1 in the present invention.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
A kind of modified carbon nitride adsorbent of manganese oxide is present embodiments provided, preparation method is specific as follows:
Step 1: 10g melamine is placed in crucible in Muffle furnace and is warming up to 550 DEG C with the heating rate of 5 DEG C/min,
2h is calcined, it is finely ground with mortar after cooling, then powder will be obtained and be placed in calcining boat in Muffle furnace with the heating of 5 DEG C/min speed
Rate is warming up to 550 DEG C, calcines 3h, obtains carbonitride；
Step 2: the four water manganese nitrates of 0.049g being added in the culture dish for filling 0.2g deionized water, are stirred with glass bar
It mixes to whole dissolutions, obtains manganese nitrate solution, the carbonitride of 0.15g is added in manganese nitrate solution, be uniformly mixing to obtain outstanding
Suspension is placed in drying box with 70 DEG C of drying 8h by supernatant liquid, and the solid abrasive being dried to obtain to 40-80 mesh then will
Obtained solid powder, which is placed in, to be burnt in boat, is sent into Muffle furnace with the heating rate of 5 DEG C/min in 200 DEG C of calcining 2h, is obtained oxygen
Change the modified carbon nitride adsorbent of manganese.
X-ray diffraction analysis (XRD) is carried out to prepared adsorbent, the adsorbent prepared as shown in Figure 2 is manganese oxide
Modified carbon nitride material.
Transmission electron microscope imaging (TEM) is made to the modified carbon nitride adsorbent of the manganese oxide of preparation, as can be seen from Figure 3 manganese oxide
There is good composite effect with carbonitride.
Embodiment 2
A kind of modified carbon nitride adsorbent of manganese oxide is present embodiments provided, preparation method is specific as follows:
Step 1: 10g melamine is placed in crucible in Muffle furnace and is warming up to 550 DEG C with the heating rate of 5 DEG C/min,
2h is calcined, it is finely ground with mortar after cooling, then powder will be obtained and be placed in calcining boat in Muffle furnace with the heating of 5 DEG C/min speed
Rate is warming up to 550 DEG C, calcines 3h, obtains carbonitride；
Step 2: the four water manganese nitrates of 0.023g being added in the culture dish for filling 0.2g deionized water, are stirred with glass bar
It mixes to whole dissolutions, obtains manganese nitrate solution, the carbonitride of 0.15g is added in manganese nitrate solution, be uniformly mixing to obtain outstanding
Suspension is placed in drying box with 70 DEG C of drying 8h by supernatant liquid, and the solid abrasive being dried to obtain to 40-80 mesh then will
Obtained solid powder, which is placed in, to be burnt in boat, is sent into Muffle furnace with the heating rate of 5 DEG C/min in 200 DEG C of calcining 2h, is obtained oxygen
Change the modified carbon nitride adsorbent of manganese.
X-ray diffraction analysis (XRD) is carried out to prepared adsorbent, the adsorbent prepared as shown in Figure 2 is manganese oxide
Modified carbon nitride material.
It is real that fixed bed flue gas mercury removal has been carried out to the modified carbon nitride material of manganese oxide prepared by embodiment 1 and embodiment 2
It tests: adsorbent prepared in 50mg embodiment is added to fixed bed evaluation test rack, be 55 μ g/ in initial mercury concentration
m3, and it is that mercury vapour under 5% oxygen, 95% nitrogen atmosphere is reacted in volume fraction under the conditions of 120 DEG C of reaction temperature, instead
The demercuration efficiency for answering embodiment 1 after 100min is 95% or so, and the demercuration efficiency of embodiment 2 removes simple substance 75% or so
The performance of mercury is apparently higher than traditional absorbent charcoal material.
Claims (7)
1. a kind of preparation method of the modified carbon nitride adsorbent of manganese oxide characterized by comprising carbonitride is added to nitric acid
In manganese solution, it is uniformly mixed and obtains suspension, move it in drying box and dry, then grind obtained solid, then by gained
Powder calcining obtains the modified carbon nitride adsorbent of manganese oxide.
2. the preparation method of the modified carbon nitride adsorbent of manganese oxide as described in claim 1, which is characterized in that the carbonitride is logical
Cross melamine with the method for secondary clacining be made, specially first by melamine be placed in crucible in Muffle furnace with 5 DEG C/
The heating rate of min is warming up to 550 DEG C, calcines 2h, then by product grinding be placed in calcining boat again in Muffle furnace with 5 DEG C/
The heating rate of min is warming up to 550 DEG C, calcines 2h to get carbonitride is arrived.
3. the preparation method of the modified carbon nitride adsorbent of manganese oxide as described in claim 1, which is characterized in that the manganese nitrate is molten
Liquid is dissolved in deionized water by four water manganese nitrates and is prepared, and the mass ratio of the carbonitride and four water manganese nitrates is
0.15:0.023~0.049.
4. the preparation method of the modified carbon nitride adsorbent of manganese oxide as described in claim 1, which is characterized in that the suspension dries
Dry temperature is 70 DEG C, and drying time is 6~8h.
5. the preparation method of the modified carbon nitride adsorbent of manganese oxide as described in claim 1, which is characterized in that the calcining is specific
Are as follows: after being warming up to 200 DEG C in Muffle furnace with the heating rate of 5 DEG C/min, calcine 2h.
6. the modified carbon nitride adsorbent of the manganese oxide of any one of Claims 1 to 5 the method preparation.
7. application of the modified carbon nitride adsorbent of manganese oxide as claimed in claim 6 in flue gas demercuration adsorbent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910410814.5A CN110115975A (en) | 2019-05-17 | 2019-05-17 | Modified carbon nitride adsorbent of a kind of manganese oxide and the preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910410814.5A CN110115975A (en) | 2019-05-17 | 2019-05-17 | Modified carbon nitride adsorbent of a kind of manganese oxide and the preparation method and application thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113042084A (en) * | 2021-03-25 | 2021-06-29 | 华东理工大学 | Preparation method and application of manganese oxide composite carbon nitride nanotube composite photocatalyst |
| CN113877618A (en) * | 2021-09-28 | 2022-01-04 | 安徽元琛环保科技股份有限公司 | Preparation method of oxygen-doped graphite-phase carbon nitride-loaded manganese-based low-temperature denitration catalyst and prepared denitration catalyst |
| CN116328712A (en) * | 2023-03-15 | 2023-06-27 | 中国舰船研究设计中心 | Novel water quality purifying composite material and preparation method and application thereof |
-
2019
- 2019-05-17 CN CN201910410814.5A patent/CN110115975A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| DONGJING LIU等: "Elemental Mercury Removal by MnO2 Nanoparticle-Decorated Carbon Nitride Nanosheet", 《ENERGY FUELS》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113042084A (en) * | 2021-03-25 | 2021-06-29 | 华东理工大学 | Preparation method and application of manganese oxide composite carbon nitride nanotube composite photocatalyst |
| CN113877618A (en) * | 2021-09-28 | 2022-01-04 | 安徽元琛环保科技股份有限公司 | Preparation method of oxygen-doped graphite-phase carbon nitride-loaded manganese-based low-temperature denitration catalyst and prepared denitration catalyst |
| CN113877618B (en) * | 2021-09-28 | 2024-01-23 | 安徽元琛环保科技股份有限公司 | Preparation method of oxygen-doped graphite-phase carbon nitride-supported manganese-based low-temperature denitration catalyst and prepared denitration catalyst |
| CN116328712A (en) * | 2023-03-15 | 2023-06-27 | 中国舰船研究设计中心 | Novel water quality purifying composite material and preparation method and application thereof |
| CN116328712B (en) * | 2023-03-15 | 2024-04-16 | 中国舰船研究设计中心 | Novel water quality purifying composite material and preparation method and application thereof |
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Application publication date: 20190813 |
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