CN109351365A - Hydrotalcite modifies g-C3N4New and effective photochemical catalyst and its application in deep desulfurization of fuel oil - Google Patents
Hydrotalcite modifies g-C3N4New and effective photochemical catalyst and its application in deep desulfurization of fuel oil Download PDFInfo
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- CN109351365A CN109351365A CN201811386575.6A CN201811386575A CN109351365A CN 109351365 A CN109351365 A CN 109351365A CN 201811386575 A CN201811386575 A CN 201811386575A CN 109351365 A CN109351365 A CN 109351365A
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- hydrotalcite
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
- C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
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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
- B01J27/24—Nitrogen compounds
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Abstract
Hydrotalcite modifies g-C3N4New and effective photochemical catalyst and its application in deep desulfurization of fuel oil, belong to environmental protection technical field.The core of this method is photochemical catalyst MN-LDHs/g-C3N4Preparation and structure regulating, be the key that improve photocatalysis efficiency, which is characterized in that first by stratiform hydrotalcite MN-LDHs growth in situ in g-C3N4Nanometer sheet is synthesized by the relative scale of both regulations with heterojunction structure, thus the photochemical catalyst for the high activity for effectively inhibiting electron-hole compound.The system is environmentally protective using air as oxidant, low in cost, and reaction condition is mild, consersion unit and simple process, and desulfurization degree 2 hours up to 95% or more, photochemical catalyst was reusable, and performance is basically unchanged, is easily recycled.
Description
Technical field
The invention belongs to environmental protection technical fields, are related to hydrotalcite/nitridation carbon composite preparation (MN-LDHs/g-
C3N4, abbreviation LDHs/g-C3N4, such as CoAl-LDHs/g-C3N4) and it is a kind of by oxidant, acetonitrile of air be extractant
Photochemical catalytic oxidation/extraction mould oil process for deep desulphurization.
Background technique
Environmental protection is the key subjects urgently to be resolved of facing mankind.With the development of economy, to the demand of cleansing oil
Constantly increase.High sulfur content fuel oil burns in air can cause a series of environmental problems, such as acid rain, haze etc..For this purpose, state
Inside and outside all to have formulated stringent regulation and policy, Europe and the U.S. just provided sulfur-bearing in 10 μ g/g hereinafter, China early in 2009
Government declared, by the control of sulfur-bearing standard in 10 μ g/g, was realized in line with international standards in 2017.1 μ g/g super-low sulfur cleaning below
Oil is following target and trend.Therefore, deep desulfuration technology becomes the research hotspot of cleaning oil tech.
Traditional hydrodesulfurization technology need under higher reaction temperature (300-400 DEG C) and pressure (3-6MPa) into
Row, largely consumes hydrogen, and be difficult to remove the thiophenes sulfides for having space steric effect in fuel oil.Absorption desulfurization, oxidation sweetening,
The beneficial complement of abstraction desulfurization and above-mentioned desulfurization combination technique as hydrodesulfurization becomes the concern of deep desulfuration technical field
Focus.Low energy consumption is researched and developed, does not consume the highly selective deep desulfuration technology of hydrogen, not only there is scientific value, but also
With great Demand of Nation and realistic meaning.
Photocatalysis and oxidation method for desulfurizing has many advantages, such as that low energy consumption, mild condition, without secondary pollution, energy deep desulfuration, standby
Paid attention to by scholar.Wherein the development of high efficiency photocatalyst is the core of the technology.By Research Literature to photocatalysis desulfurization and
The tracking of patent finds graphite phase carbon nitride (g-C3N4) the good photocatalysis performance that has of semiconductor material.g-C3N4Material
With lot of advantages, such as: it is at low cost, abundance, nontoxic.These advantages cause researchers and optimize its photocatalysis performance
Interest.With g-C3N4It is similar, hydrotalcite-based compound because of its preferable photocatalysis performance and its controllable electronic structure, also by
It is widely used as the constituent element of composite photo-catalyst.Hydrotalcite is a kind of novel green catalyst, has main layer board metallic element group
At can modulation, the regulatable feature of the anion intercalated the Nomenclature Composition and Structure of Complexes of object is expected to form various structures, and powerful is compound
Multifunctional material or will show wide in many fields such as absorption, catalysis, medicine, electrochemistry, photochemistry, magnetic material
Wealthy application prospect.According to literature research, it is feasible for developing hydrotalcite-like material as photochemical catalyst.Hydrotalcite and g-C3N4It is multiple
Condensation material has excellent photocatalysis performance, and there may be electronics synergistic effects for two kinds of storerooms, and it is compound to reduce electron-hole
Rate, which are mainly applied to the work in terms of photodissociation aquatic products hydrogen and degradation of dye, and applied to photochemical catalytic oxidation desulfurization to have no at present
Report.
Summary of the invention
The purpose of the present invention is to provide a kind of novel photocatalysts cheap and easy to get, that is, prepare different types of LDHs/
g-C3N4Material, for the sulfur-containing compound in photochemical catalytic oxidation removing fuel oil.Building air is oxidant, and acetonitrile is extractant
Environmentally protective deep desulfuration new system.
LDHs/g-C of the invention3N4, under normal temperature and pressure conditions, using air as oxidant, ultraviolet lamp is light source, and light is urged
The sulfurous organic compound changed in model of oxidation oil becomes the stronger sulfone of polarity, is extracted with acetonitrile extraction agent, to remove containing in oil
Sulfur organic obtains super-low sulfur cleansing oil.
Hydrotalcite of the invention modifies g-C3N4Photochemical catalyst, which is characterized in that hydrotalcite and g-C3N4It is combined with each other,
Stratiform hydrotalcite MN-LDHs growth in situ is in g-C3N4In nanometer sheet, wherein mass percent 10%-70% shared by hydrotalcite.
Hydrotalcite of the present invention modifies g-C3N4The preparation of photochemical catalyst, which is characterized in that the technical solution packet of use
Include following steps:
(1) thermal polymerization method prepares graphite phase carbon nitride g-C3N4；
Wherein step (1) is conventional method, weighs a certain amount of urea and is placed in crucible with a lid, places it in Muffle furnace
Middle calcining rises to 500-550 DEG C with the heating rate of 2.3-20 DEG C/min, keeps the temperature a few hours；Subsequent Temperature fall, grinding, obtains
To target material.
(2) in-situ synthesis prepares MN-LDHs/g-C3N4Composite material
Weigh the g-C of step (1) preparation3N4, be placed in water heating kettle, weigh it is a certain amount of prepare hydrotalcite needed for divalent
Metal M nitrate and trivalent metal N nitrate, which are added in aqueous solution, is placed in water heating kettle, then by water heating kettle ultrasound 30min, ultrasound
Water heating kettle is placed in aging in 110 DEG C of baking ovens by precipitating reagent needed for addition prepares hydrotalcite afterwards, washs later, is dry, grinding
To target material.
Divalent metal nitrate and trivalent metal nitrate molar ratio are (1-4) in step (2) colloidal sol: 1, preferably 3:1 or
2:1。
Wherein divalent metal M nitrate includes but is not limited to cobalt nitrate, zinc nitrate；Trivalent metal N nitrate includes but not
It is limited to aluminum nitrate, chromic nitrate.
The precipitating reagent is urea or/sodium hydroxide and sodium carbonate etc..
The invention also discloses the catalyst to be used for fuel desulfuration.
A kind of photocatalysis deep desulfurization of fuel oil system, which is characterized in that with the hydrotalcite/nitridation carbon composite
MN-LDHs/g-C3N4As photochemical catalyst, using air as oxidant, catalytic desulfurization is carried out to fuel oil under ultraviolet light irradiation,
The sulphur product generated simultaneously using acetonitrile as solvent extraction reaction.
The method that the above-mentioned desulfurization system of the present invention carries out photocatalysis desulfurization: the above-mentioned photochemical catalyst of preparation is added to be desulfurization
System (as oil) in, be passed through air, under ultraviolet light irradiation, react a few hours, while using acetonitrile extraction；Sulphur blood urea/nitrogen analyzer
Analyze its desulfurization degree.
Acetonitrile: fuel oil system volume ratio=1:1-1:1.5 to be desulfurization.The sulfur material contained in fuel oil system to be desulfurization
For at least one of BT, DBT, 4,6-DMDBT.
Light-catalyzed reaction of the present invention 2 hours, desulfurization degree are about 95%-100%, and repeated experiment proves that catalyst performance is steady
It is fixed.
The present invention provides in-situ synthesis to prepare CoAl-LDHs/g-C3N4Photochemical catalyst, and it is de- for photocatalysis depth
The method of sulphur.The catalyst raw material is cheap and easy to get, and reaction condition is mild, and consersion unit and simple process, catalyst are urged with light
Change the high and reusable feature of activity.It is important that this method finds that hydrotalcite-like material has in photocatalysis deep desulfuration field
Application value, it is with important application prospects also to provide new approaches by the process for deep desulphurization of oxidant of air.The party
The core of method is photochemical catalyst MN-LDHs/g-C3N4Preparation and structure regulating, be the key that improve photocatalysis efficiency, first will
Stratiform hydrotalcite MN-LDHs growth in situ is in g-C3N4Nanometer sheet is synthesized by the relative scale of both regulations with heterogeneous
Structure, thus the photochemical catalyst for the high activity for effectively inhibiting electron-hole compound.The system is using air as oxidant, green ring
It protects, low in cost, reaction condition is mild, consersion unit and simple process, and desulfurization degree 2 hours up to 95% or more, photochemical catalyst could
It reuses, and performance is basically unchanged, is easily recycled.
Detailed description of the invention
The electron microscope (SEM) of 1 material prepared of Fig. 1 embodiment.
(a) scanning electron microscope (SEM) photograph (b) 20%LDHs/g-C of CoAl-LDHs3N4Scanning electron microscope (SEM) photograph；
The transmission electron microscope picture (TEM) of 1 material prepared of Fig. 2 embodiment.
The X-ray diffractogram (XRD) of Fig. 3 material prepared.
The infrared analysis figure (FTIR) of Fig. 4 material prepared.
(a)CoAl-LDHs；(b) 20%CoAl-LDHs/g-C3N4；(c)g-C3N4
Specific embodiment
Illustrated embodiment is preference below, should be not limited to following instance in practical applications.
Embodiment 1:CoAl-LDHs/g-C3N4Preparation and photocatalysis performance
(1) thermal polymerization method prepares g-C3N4
It weighs 20g urea to be placed in crucible with a lid, places it in Muffle furnace and calcine, with the heating speed of 20 DEG C/min
Rate rises to 500 DEG C, keeps the temperature 2 hours, then rises to 520 DEG C with the heating rate of 20 DEG C/min, keeps the temperature 2 hours.Subsequent Temperature fall,
Grinding, obtains target material.
(2)CoAl-LDHs/g-C3N4Preparation
Weigh 0.5g g-C3N4, be scattered in 80mL water and be placed in 80mL water heating kettle, weigh 0.2725g cobalt nitrate and
0.1175g aluminum nitrate (molar ratio 3:1) is added into water heating kettle.Then by water heating kettle ultrasound 30min, 0.225g is added after ultrasonic
Water heating kettle is placed in aging 16h in 110 DEG C of baking ovens by urea, washs later, is dry, grinding to obtain target material.
(3) mould oil is prepared
It weighs 0.1856g DBT to be dissolved in 90mL normal octane, the mould oil that sulfur content is 500ppm is made；It weighs
0.1362g BT is dissolved in 90mL normal octane, and the mould oil that sulfur content is 500ppm is made；It is molten to weigh 0.2142g 4,6-DMDBT
In 90mL normal octane, the mould oil that sulfur content is 500ppm is made.
(4) photochemical catalytic oxidation desulfurization
Take 90mL mould oil (500ppm DBT), 90mL acetonitrile and 0.09g CoAl-LDHs/g-C3N4It is added to reactor
In, it is stirred in dark and reaches within 0.5 hour adsorption equilibrium, air mass flow is under 25mL/min, and after illumination reaction 2h, sulfur content is
19.5ppm, desulfurization degree is up to 96.1%；DBT in mould oil is changed to BT, and when keeping sulfur content identical, desulfurization degree is reachable
100%；DBT in mould oil is changed to 4,6DMDBT, and when keeping sulfur content identical, desulfurization degree is up to 95.8%.
From XRD diagram it is found that the CoAl-LDHs/g-C prepared3N4Material, with the continuous improvement of hydrotalcite component content,
Hydrotalcite diffraction maximum constantly becomes by force, and g-C3N4Diffraction maximum die down.Both but can significantly observe in the composite
Characteristic peak, this shows g-C3N4Growth of the presence without influence on hydrotalcite crystal, and g-C in the synthesis process3N4Knot
Structure also there is no variation, successfully prepares CoAl-LDHs/g-C3N4Composite material.FTIR map further proves to have succeeded
Synthesized CoAl-LDHs/g-C3N4Composite material.
Shown by electron microscope: in CoAl-LDHs/g-C3N4In composite material, the surface of CoAl-LDHs is by g-C3N4Piece covers
Lid shows a kind of sheet stacking pattern.g-C3N4It is made of the nano-plates of many curved, irregular and uneven sizes.
These features show to interact by electrostatical binding or electric charge transfer, and there are very strong phase interactions between two kinds of layer package materials
With.
Embodiment 2:ZnAl-LDHs/g-C3N4Preparation and its photocatalysis performance
(1) thermal polymerization method prepares g-C3N4
It weighs 20g urea to be placed in crucible with a lid, places it in Muffle furnace and calcine, with the heating speed of 20 DEG C/min
Rate rises to 500 DEG C, keeps the temperature 2 hours, then rises to 520 DEG C with the heating rate of 20 DEG C/min, keeps the temperature 2 hours.Subsequent Temperature fall,
Grinding, obtains target material.
(2)ZnAl-LDHs/g-C3N4Preparation
Weigh 0.6g g-C3N4, it is added in the four-hole bottle equipped with 100mL water, ultrasonic 30min.Weigh 2.975g Zn
(NO3)2, 1.876g Al (NO3)3It is dissolved in 100mL deionized water, then weighs 1.2g NaOH, 0.536g Na2CO3It is dissolved in
In 100mL deionized water, salting liquid and aqueous slkali are instilled in four-hole bottle simultaneously later, and keeping pH value is 10, titration finishes
It keeps for 24 hours for 80 DEG C afterwards.Whole process holding is vigorously stirred, and is filtered, and is washed, dry, and grinding obtains target sample.
(3) photochemical catalytic oxidation desulfurization
Take 90mL mould oil, 90mL acetonitrile and 0.18g ZnAl-LDHs/g-C3N4It is added in reactor, is stirred in dark
Reach within 0.5 hour adsorption equilibrium, air mass flow is under 25mL/min, and after illumination reaction 2h, sulfur content is reduced to 20ppm, desulfurization degree
Up to 96%.
Embodiment 3:ZnCr-LDHs/g-C3N4Preparation and its photocatalysis performance
(1) thermal polymerization method prepares g-C3N4
It weighs 20g urea to be placed in crucible with a lid, places it in Muffle furnace and calcine, with the heating speed of 20 DEG C/min
Rate rises to 500 DEG C, keeps the temperature 2 hours, then rises to 520 DEG C with the heating rate of 20 DEG C/min, keeps the temperature 2 hours.Subsequent Temperature fall,
Grinding, obtains target material.
(2)ZnCr-LDHs/g-C3N4Preparation
Weigh 1g g-C3N4, it is added in the beaker equipped with 80mL water, ultrasonic 30min.Weigh 5.951g Zn (NO3)2,
4.002g Cr(NO3)3It is dissolved in 100mL deionized water, is added dropwise to g-C3N4In dispersion liquid, then to weigh 2.4g NaOH molten
In 60mL deionized water, NaOH solution is instilled in beaker later, pH value is adjusted to 5.5, continues stirring half after titration
Hour, it filters, washs later, dry, grinding obtains target sample.
(3) photochemical catalytic oxidation desulfurization
Take 90mL mould oil, 90mL acetonitrile and 0.18g ZnCr-LDHs/g-C3N4It is added in reactor, is stirred in dark
Reach within 0.5 hour adsorption equilibrium, under the conditions of air mass flow is 25mL/min, after illumination reaction 2h, sulfur content is reduced to 25ppm, takes off
Sulphur rate is up to 95%.
Claims (10)
1. hydrotalcite modifies g-C3N4Photochemical catalyst, which is characterized in that hydrotalcite and g-C3N4It is combined with each other, stratiform hydrotalcite
MN-LDHs growth in situ is in g-C3N4In nanometer sheet, wherein mass percent shared by hydrotalcite is 10%-70%.
2. preparing hydrotalcite modification g-C described in claim 13N4The method of photochemical catalyst, which is characterized in that including following step
It is rapid:
(1) thermal polymerization method prepares graphite phase carbon nitride g-C3N4；
(2) in-situ synthesis prepares MN-LDHs/g-C3N4Composite material
Weigh the g-C of step (1) preparation3N4, be placed in water heating kettle, weigh it is a certain amount of prepare hydrotalcite needed for divalent metal M
Nitrate and trivalent metal N nitrate, which are added in aqueous solution, to be placed in water heating kettle, then by water heating kettle ultrasound 30min, after ultrasonic
Water heating kettle is placed in aging in 110 DEG C of baking ovens by precipitating reagent needed for addition prepares hydrotalcite, washs later, is dry, grinding to obtain mesh
Mark material.
3. according to the method for claim 2, which is characterized in that divalent metal nitrate and trivalent gold in step (2) colloidal sol
Genus nitrobacter molar ratio is (1-4): 1.
4. according to the method for claim 2, which is characterized in that divalent metal nitrate and trivalent metal nitrate molar ratio
For 3:1 or 2:1.
5. according to the method for claim 2, which is characterized in that divalent metal M nitrate is selected from cobalt nitrate, zinc nitrate；Three
Valence metal N nitrate is selected from aluminum nitrate, chromic nitrate.
6. according to the method for claim 2, which is characterized in that the precipitating reagent is urea or sodium hydroxide and carbonic acid
Sodium.
7. hydrotalcite described in claim 1 modifies g-C3N4The application of photochemical catalyst is used for fuel desulfuration.
8. a kind of photocatalysis deep desulfurization of fuel oil system, which is characterized in that modify g- using hydrotalcite described in claim 1
C3N4Photochemical catalyst carries out catalytic desulfurization to fuel oil under ultraviolet light irradiation, while making using acetonitrile using air as oxidant
The sulphur product generated for solvent extraction reaction.
9. system according to claim 7, which is characterized in that acetonitrile: fuel oil system volume ratio=1:1-1 to be desulfurization:
1.5。
10. system according to claim 7, which is characterized in that the sulfur material contained in fuel oil system to be desulfurization be BT,
At least one of DBT, 4,6DMDBT.
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| CN110270364A (en) * | 2019-07-16 | 2019-09-24 | 河北工业大学 | A kind of support type graphite phase carbon nitride composite material, preparation method and applications |
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| CN110813313A (en) * | 2019-11-11 | 2020-02-21 | 安徽理工大学 | Silver oxide/layered double-metal hydroxide compound and preparation and application thereof |
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| CN111167499A (en) * | 2020-01-21 | 2020-05-19 | 佛山科学技术学院 | NiM-LDH/g-C3N4Composite photocatalytic material and preparation method thereof |
| CN111545235A (en) * | 2020-04-23 | 2020-08-18 | 宁德师范学院 | 2D/2Dg-C3N4CoAl-LDH hydrogen-production heterojunction material and preparation method and application thereof |
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| CN111912887B (en) * | 2020-06-22 | 2023-02-17 | 江苏中江材料技术研究院有限公司 | Preparation method of photoelectrochemical ofloxacin aptamer sensor based on hydrotalcite/graphite-like phase carbon nitride heterojunction |
| CN114984991A (en) * | 2022-05-24 | 2022-09-02 | 浙江微通催化新材料有限公司 | g-C 3 N 4 Preparation method of modified hydrotalcite catalyst and application of modified hydrotalcite catalyst in condensation reaction of furfural and cyclic ketone |
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