CN109731602A - Surfactant/UiO-66-NH2Composite photo-catalyst and preparation method thereof - Google Patents
Surfactant/UiO-66-NH2Composite photo-catalyst and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of surfactant/UiO-66-NH2The preparation method of composite photo-catalyst, comprising the following steps: S1, ZrCl4It is dissolved in n,N-Dimethylformamide with 2- amino terephthalic acid (TPA) and forms mixture, wherein volume content is 30~40% to the n,N-Dimethylformamide in the mixture, the molar content of the 2- amino terephthalic acid (TPA) and the ZrCl4Molar content it is equal；The mixture is heated to 115 DEG C~125 DEG C reactions, obtains yellow solid product after cooling by S2；The yellow solid product is centrifugated by S3, and is exchanged washing with methanol and removed product UiO-66-NH2Remaining DMF in duct, finally vacuum drying obtains UiO-66-NH2Sample；S4, by SURFACTANT ADSORPTION in the UiO-66-NH2In sample, surfactant/UiO-66-NH is formed2Composite photo-catalyst.The present invention also provides one kind surfactant made of the above method/UiO-66-NH2Composite photo-catalyst.
Description
Technical field
The present invention relates to a kind of surfactant/UiO-66-NH2Composite photo-catalyst and preparation method thereof.
Background technique
Photocatalysis technology is the one of which of high-level oxidation technology, and most of organic pollutants difficult to degrade are all to pass through life
At active oxidation substance just remove, therefore cause the people extremely to pay close attention to this field and expectation.Photocatalysis depollution of environment skill
Art be using the electrons and holes formed in the active material of high redox potential, light-catalyzed reaction to and environmental system in have
Reach basic degradation and machine object and inorganic compound are all the chemical bonds by destroying them.Therefore, this technology is caused to exist
There is many advantages for the purification of application environment: lower cost, security performance are high, the nontoxic nothing of catalyst itself utilized
It is harmful, environment purification is high-efficient and also possesses potentiality for excavating solar energy and expansionary strong etc..
Although MOFs material has many advantages, such as, but the application in photocatalysis field is still limited, and is extended new
MOFs material is abundant and necessary task.The thermal stability of MOFs material is lower, and generally at 350~400 DEG C, but UiO-66 has
There is the stability of superelevation, structure collapse temperature is greater than or equal to 500 DEG C, and UiO-66 is in irregular little particle, and chemical formula is
Zr6O4(OH)4(CO2)12, the three-dimensional structure for being formed by tetrahedron and octahedra two types hole cage is by Zr6Regular octahedron with
12 terephthalic acid (TPA) ligands are connected, and have good water-resistance and antacid excellent properties.In view of UiO-66 only has purple
Outer absorbing properties introduce amido functional group in its ligand, have obtained its isomorphism and spread out using simple " preceding functionalization " method
Biological UiO-66 (NH2)。UiO-66-NH2It may be regarded as based semiconductor material, issue raw electron transition in visible light action, generate
Electron-hole pair, the V of Preventing coughfbAbout -0.8V (vs Ag/AgCl) is lower than O2 -/O2(- 0.28eV), conduction band potential is about
1.95V(vs Ag/AgCl)。UiO-66-NH2With strong oxidizing property, it is adsorbed on the OH on catalyst particle surface layer-Or H2O is by oxygen
It is melted into hydroxyl radical free radical.The reactivity of hydroxyl radical free radical is very high, can aoxidize a small number of inorganic matter and most of organic matter,
It is set to be converted into the CO of environmental sound2And H2O.Light induced electron can be with the O that is adsorbed on photocatalyst surface2Oxidation reaction occurs
And generate superoxide radical O2 -, realize the reduction to organic matter and inorganic matter.
But UiO-66-NH2It is easy to reunite between each other when carrying out light-catalyzed reaction, can not uniformly be scattered in mould
In quasi- fuel oil system.
Summary of the invention
The present invention provides a kind of surfactant/UiO-66-NH2Composite photo-catalyst and preparation method thereof, Ke Yiyou
Effect solves the above problems.
The present invention is implemented as follows:
A kind of surfactant/UiO-66-NH2The preparation method of composite photo-catalyst, comprising the following steps:
S1, ZrCl4It is dissolved in n,N-Dimethylformamide with 2- amino terephthalic acid (TPA) and forms mixture, wherein institute
Stating n,N-Dimethylformamide, volume content is 30~40% in the mixture, the molar content of the 2- amino terephthalic acid (TPA)
With the ZrCl4Molar content it is equal；
The mixture is heated to 115 DEG C~125 DEG C reactions, obtains yellow solid product after cooling by S2；
The yellow solid product is centrifugated by S3, and is exchanged washing with methanol and removed product UiO-66-NH2Duct
Interior remaining DMF, finally vacuum drying obtains UiO-66-NH2Sample；
S4, by SURFACTANT ADSORPTION in the UiO-66-NH2In sample, surfactant/UiO-66-NH is formed2It is multiple
Light combination catalyst.
The present invention also provides a kind of surfactant/UiO-66-NH obtained by the above method2Composite photo-catalyst.
The beneficial effects of the present invention are: the present invention is by surfactant to UiO-66-NH2Granular system is modified, from
And it avoids being easy aggregation agglomerating the technical issues of causing photocatalysis efficiency to reduce between particle, and further increase UiO-66-NH2
Lipophilic and photocatalysis efficiency.
Detailed description of the invention
It, below will be to use required in embodiment in order to illustrate more clearly of the technical solution of embodiment of the present invention
Attached drawing be briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not to be seen as
It is the restriction to range, it for those of ordinary skill in the art, without creative efforts, can be with root
Other relevant attached drawings are obtained according to these attached drawings.
That Fig. 1 is shown is 10mg 0.5%SDS/UiO-66-NH respectively2, 20mg 0.5%SDS/UiO-66-NH2And 40mg
0.5%SDS/UiO-66-NH2Be scattered in pyridine adsorption performance map.
Fig. 2 is various concentration SDS/UiO-66-NH2Fuel oil denitrogenation figure.
That Fig. 3 is shown is 10mg 0.5%SHS/UiO-66-NH respectively2, 20mg 0.5%SHS/UiO-66-NH2And 40mg
0.5%SHS/UiO-66-NH2Be scattered in pyridine adsorption performance map.
Fig. 4 is various concentration SHS/UiO-66-NH2Fuel oil denitrogenation figure.
Specific embodiment
To keep the purposes, technical schemes and advantages of embodiment of the present invention clearer, implement below in conjunction with the present invention
The technical solution in embodiment of the present invention is clearly and completely described in attached drawing in mode, it is clear that described reality
The mode of applying is some embodiments of the invention, rather than whole embodiments.Based on the embodiment in the present invention, ability
Domain those of ordinary skill every other embodiment obtained without creative efforts, belongs to the present invention
The range of protection.Therefore, the detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit below and is wanted
The scope of the present invention of protection is sought, but is merely representative of selected embodiment of the invention.Based on the embodiment in the present invention,
Every other embodiment obtained by those of ordinary skill in the art without making creative efforts belongs to this
Invent the range of protection.
In the description of the present invention, term " first ", " second " are used for description purposes only, and should not be understood as instruction or dark
Show relative importance or implicitly indicates the quantity of indicated technical characteristic.The feature of " first ", " second " is defined as a result,
It can explicitly or implicitly include one or more of the features.In the description of the present invention, the meaning of " plurality " is two
It is a or more than two, unless otherwise specifically defined.
Embodiment A1~A4:
Zirconium chloride (233.2mg, about 1.0mmol), which is first dissolved in 50mL N-N- dimethylformamide, to be stirred after five minutes, then plus
Enter 1.0mmol 181.2mg 2- amino para Toluic Acid, the autoclave of 30mL is gone to after magnetic stirrer 1 hour
In, it finally puts baking oven into, is reacted 48 hours at 120 DEG C.Sample natural cooling after reaction, drops to room temperature, by clear liquid (N-N- bis-
Methyl nitrosourea) it pours into special waste liquid bottle.UiO-66-NH2The same day of synthesis is centrifuged three times, then every 24 hours from
The heart is primary (in total 3 times).It finally puts Centrifuge Cup into vacuum drying oven drying, obtains final sample UiO-66-NH2.Take 0.1g
Obtained UiO-66-NH2Sample dispersion is in 30mL deionized water, ultrasonic 2min, and be separately added into 0.5mL, 1mL, 2mL,
The SDS surfactant solution of the 0.25g/L of 4mL, stirring and adsorbing 1h.After, with the high speed centrifugation of 8000r/min revolving speed
Machine is centrifuged 10min, then uses deionized water supersound washing, is then centrifuged 2 times, is placed in freeze-day with constant temperature 6h in baking oven (80 DEG C), then
It is 0.125% that freeze-day with constant temperature 12h, which is placed in vacuum drying oven (80 DEG C), to get load factor, 0.25%, 0.5%, 1% SDS/
UiO-66-NH2Composite photo-catalyst is denoted as 0.125%SDS/UiO-66-NH2(B1), 0.25%SDS/UiO-66-NH2(B2)、
0.5%SDS/UiO-66-NH2(B3), 1%SDS/UiO-66-NH2(B4)。
Embodiment B1~B4:
By the ZrCl of 0.2332g4(1.0mmol) is added in the hydrothermal reaction kettle of 100mL, then measures 50mL N, N- bis-
Methylformamide (DMF) is added thereto, and stirring 5min makes it completely dissolved, and adds the 2- amino terephthalic acid (TPA) of 0.1812g
After (1.0mmol) is stirred 1 hour, reaction kettle is placed in stainless steel steel bushing and is screwed, reacts 48h at 120 DEG C.After reaction to
Sample cooled to room temperature takes out reaction kettle, yellow solid product obtained in reaction is transferred in Centrifuge Cup, methanol is added
Centrifugation, and with methanol exchange washing for several times (6-7 times) to completely removing product UiO-66-NH2Remaining DMF in duct, finally
Solid product is placed in freeze-day with constant temperature at 100 DEG C of vacuum, obtained sample is UiO-66-NH2.It takes obtained by 0.1g
UiO-66-NH2Sample dispersion is in 30mL deionized water, ultrasonic 2min, and is separately added into 0.5mL, 1mL, 2mL, 4mL
The SHS surfactant solution of 0.25g/L, stirring and adsorbing 1h.After, with the supercentrifuge of 8000r/min revolving speed from
Then heart 10min uses deionized water supersound washing, be then centrifuged 2 times, be placed in freeze-day with constant temperature 6h in baking oven (80 DEG C), then be placed in
Freeze-day with constant temperature 12h is 0.125% to get load factor in vacuum drying oven (80 DEG C), 0.25%, 0.5%, 1% SHS/UiO-66-
NH2Composite photo-catalyst is denoted as 0.125%SHS/UiO-66-NH2(B1), 0.25%SHS/UiO-66-NH2(B2), 0.5%
SHS/UiO-66-NH2(B3), 1%SHS/UiO-66-NH2(B4)。
SDS/UiO-66-NH2The absorption property of catalyst and fuel oil denitrogenation analysis:
That Fig. 1 is shown is 10mg 0.5%SDS/UiO-66-NH respectively2, 20mg 0.5%SDS/UiO-66-NH2And 40mg
0.5%SDS/UiO-66-NH2Be scattered in pyridine adsorption performance map.From Fig. 1 we can see that in SDS/UiO-66-NH2
Composite photo-catalyst is all the SDS/UiO-66-NH in 3h to 4h in downward trend in 0h to 2h2Composite photo-catalyst all reaches
Adsorption equilibrium is arrived.From Fig. 1, we can also be seen that 10mg 0.5%SDS/UiO-66-NH2Adsorption rate only has 11%, absorption effect
Fruit is relatively low.And 40mg 0.5%SDS/UiO-66-NH2Adsorption rate is 15%, and adsorption effect is higher, therefore we obtain carry out light
The best sample injected volume of Catalysis experiments is 20mg.
Fig. 2 can be seen that the surfactant of various concentration has a certain impact to composite photo-catalyst activity obtained,
When SDS load factor increases to 0.25% by 0.125%, when catalyst activity increase, it is seen that fuel oil after light illumination 240min
Denitrification percent is up to 45% or more.When SDS concentration continues to be gradually increased, the activity of composite photocatalyst sample obtained is constantly risen
Height, when use SDS load factor be 0.5% sample as photochemical catalyst (0.5%SDS/UiO-66-NH2) when, activity is most
Height, fuel oil denitrification percent are up to 52% or more.However, when SDS concentration continues to be gradually increased, composite photocatalyst sample obtained
Activity reduce, when use SDS load factor for 1% sample as photochemical catalyst (1%SDS/UiO-66-NH2) when, fuel oil denitrogenation
Rate is only 42%.This may be to form organic layer as caused by excessive SDS load " screen effect ", hinder reaction bottom
Object pyridine is directly contacted with photochemical catalyst, leads to active reduction.Experiments have shown that 20mg 0.5%SDS/UiO-66-NH2It is compound
Photochemical catalyst is the optimal selection of fuel oil denitrification percent.
SHS/UiO-66-NH2The analysis of photocatalysis fuel oil denitrogenation:
One of an important factor for amount of photochemical catalyst is influence catalytic activity, Fig. 3 are the 0.5%SHS/UiO- of different amounts
66-NH2To simulation fuel oil adsorption rate, from the figure 3, it may be seen that with 0.5%SHS/UiO-66-NH2The increase of dosage, pyridine adsorption
Rate also increases.Quality is respectively that adsorption rate corresponding to 10mg, 20mg, 40mg is respectively 25%, 32%, 40%.And because
The catalytic effect of 10mg is poor, and the adsorption rate of 40mg is excessively high, therefore selects the photochemical catalyst of 20mg as the best of experimental study
Dosage.
As shown in figure 4, the SHS of various concentration is surfactant modified to UiO-66-NH2Photocatalysis nitrogen removal performance has one
Fixing is rung.The UiO-66-NH of unsupported sample2Activity it is poor, pyridine denitrification percent after illumination 4h is 30%.It is dense with loading
The activity of the increase of degree, composite catalyst increases, SHS/UiO-66-NH when reaching 0.5%2Activity it is maximum, after illumination 4h
Denitrification percent reaches 60%, but activity is declined when concentration increases to 1%, this may be to make due to loading excessive SHS
At " screen effect ", form certain thickness organic layer, hinder directly contacting for reaction substrate pyridine and photochemical catalyst, lead
Activation reduces.
The foregoing is merely the preferred embodiment of the present invention, are not intended to restrict the invention, for this field
For technical staff, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any
Modification, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of surfactant/UiO-66-NH2The preparation method of composite photo-catalyst, which comprises the following steps:
S1, ZrCl4It is dissolved in n,N-Dimethylformamide with 2- amino terephthalic acid (TPA) and forms mixture, wherein the N, N-
Dimethylformamide in the mixture volume content be 30~40%, the molar content of the 2- amino terephthalic acid (TPA) with it is described
ZrCl4Molar content it is equal；
The mixture is heated to 115 DEG C~125 DEG C reactions, obtains yellow solid product after cooling by S2；
The yellow solid product is centrifugated by S3, and is exchanged washing with methanol and removed product UiO-66-NH2It is remained in duct
DMF, finally vacuum drying obtain UiO-66-NH2Sample；
S4, by SURFACTANT ADSORPTION in the UiO-66-NH2In sample, surfactant/UiO-66-NH is formed2Complex light
Catalyst.
2. preparation method according to claim 1, which is characterized in that in step s 2, the mixture is heated to 120
DEG C reaction 45~50 hours.
3. preparation method according to claim 1, which is characterized in that in step s3, with methanol exchange washing 5~8 times
To remove product UiO-66-NH2Remaining DMF in duct.
4. preparation method according to claim 1, which is characterized in that in step s 4, described to include by surfactant
SHS, SDS and its mixture.
5. preparation method according to claim 1, which is characterized in that in step s 4, described by SURFACTANT ADSORPTION
In the UiO-66-NH2Step in sample includes:
S41, by 0.1g UiO-66-NH2Sample dispersion is in 30mL deionized water, ultrasonic disperse, and SHS surfactant is added
Solution, high speed centrifugation after stirring and adsorbing；Then deionized water supersound washing is used, and is centrifuged, last vacuum drying.
6. preparation method according to claim 1, which is characterized in that in step s 4, described by SURFACTANT ADSORPTION
In the UiO-66-NH2Step in sample includes:
S41, by UiO-66-NH2Surfactant solution is added in deionized water in sample dispersion, after stirring and adsorbing high speed from
The heart；Then deionized water supersound washing is used, and is centrifuged, last vacuum drying.
7. preparation method according to claim 6, which is characterized in that in step S41, the surfactant with it is described
UiO-66-NH2The mass ratio of sample is 0.1~2:100.
8. a kind of surfactant/UiO-66-NH2Composite photo-catalyst, which is characterized in that the surfactant/UiO-66-
NH2Composite photo-catalyst is prepared by the method for any one of claim 1-7.
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Cited By (1)
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