CN109589934A - It is adjusted based on benzoic acid and chloroform activates the method and adsorption applications for preparing UiO-66 - Google Patents
It is adjusted based on benzoic acid and chloroform activates the method and adsorption applications for preparing UiO-66 Download PDFInfo
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- CN109589934A CN109589934A CN201811521854.9A CN201811521854A CN109589934A CN 109589934 A CN109589934 A CN 109589934A CN 201811521854 A CN201811521854 A CN 201811521854A CN 109589934 A CN109589934 A CN 109589934A
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
- B01J20/226—Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The invention belongs to environmental material field, the method and its adsorption applications for adjusting based on benzoic acid and preparing UiO-66 with chloroform activation are disclosed.The present invention successfully synthesizes the UiO-66 (UiO-66-BA) with perfect vertical octahedral structure as activator as regulator and chloroform by benzoic acid, and it uses X-ray diffraction (XRD), infrared figure of Fourier (FTIR) etc. proves.Absorption congo red (CR) experiment shows that the UiO-66-BA material for adding benzoic acid and chloroform has a very efficient absorption property, maximal absorptive capacity 1371mg/g, be under the same terms unmodified UiO-66 to 7 times of CR adsorbance.The present invention provides important benchmark for MOF fine synthesis nano structural material, to adjust material crystals pattern and improve the absorption property of material, thus preferably degradable organic pollutant.
Description
Technical field
The technical field of environmental contaminants is prepared and its removed the invention belongs to nanocomposite and environmentally conscious materials, is related to
A kind of in-situ method preparation perfection crystalline form UiO-66 material (UiO-66-BA) and its performance study of acid adjusting and chloroform activation.
Background technique
The transition metal ions network that metal organic framework (MOFs) representative is connected by organic ligand forms novel microporous
Material.Since MOF has high surface area, the characteristic of high porosity and adjustability, therefore it is considered as gas storage, absorbs, it is micro-
The potential candidate of electronics and catalysis.In MOFs race, Zr6O4(OH)4With 1,4- terephthalic acid (TPA) (H2BDC) connector forms 12
It is coordinated highly-filled face-centered cubic (fcc) structure (the highest report coordination of MOF), so that Zr base MOFs (UiO-66) has solely
Special performance, such as rare water stability, excellent thermal stability and chemical stability, can under strong acid and strong alkali environment
Keep high stability.Due under strong acid and strong alkali environment there is water stability and excellent chemical stability, UiO-66 to have succeeded
For liquid phase adsorption.However, traditional synthesis UiO-66 has the shortcomings that, such as low surface area, small-bore influences macromolecular dye
The absorption of material, the fault of construction of UiO-66 influence its hydrophobicity.It is well known that the appropriate selection of synthesis condition and activation process can
In the form of controlling and adjust UiO-66 and structure.Lee et al. has obtained UiO-66 by the way that the Microwave-assisted synthesis of acetic acid is added,
Prove that UiO-66 can adsorb charged dye.Qiu et al. prepares acid promotion with acetic acid or hydrochloric acid under various reaction conditions
UiO-66, and anionic dye (methyl orange and Congo red) and the dye of positive ion (methylene blue and rhodamine B) are selected
Property absorption.Azhar etc. has found the UiO-66 of chloroform activation, greatly improves it to the absorption property of sulfonamides antibiotic.Always
It, it can be seen that the synthesis and activation process that acid promotes can effectively improve crystal structure, to obtain preferably absorption effect
Fruit.
Summary of the invention:
The purpose of the present invention is to provide the preparations adjusted based on benzoic acid with the UiO-66 (UiO-66-BA) of chloroform activation
Benzoic acid is adjusted and chloroform activation collaboration is got up, is more advantageous to and improve material specific surface area etc. by method and its performance study
Correlated performance makes it have good adsorption capacity.
In order to achieve the above purpose, present invention employs technical solutions below:
Benzoic acid adjusts and the preparation method of UiO-66 (UiO-66-BA) material of chloroform activation, comprising the following steps:
(1) by ZrCl4, H2BDC and benzoic acid are dissolved in DMF solution, are poured into after mixing evenly equipped in polytetrafluoroethylene (PTFE)
In the stainless steel autoclave of lining.Wherein ZrCl4: H2BDC: the molar ratio of benzoic acid is 1:1:30.
(2) then reaction kettle is placed in air dry oven and is heated 24 hours with 120 DEG C, after reaction kettle is cooled to room temperature
Centrifugation obtains white crystal.
(3) by obtained white crystal with DMF and methanol wash three times afterwards immerse methanol solution in and in a kettle,
100 DEG C are handled 12 hours, are filtered after processing, and filter cake is washed, and drying obtains powder.
(4) above-mentioned powder is immersed in chloroform 5 days, filters, obtains sample and be centrifuged with methanol, collected lower sediment, finally exist
UiO-66 material (the UiO-66- activated with chloroform is adjusted based on benzoic acid to obtain within drying 12 hours for 100 DEG C in vacuum drying oven
BA)。
The UiO-66-BA material obtained has perfectly vertical octahedral structure, has big specific surface area, improves it
Adsorption capacity can be used as adsorbent for removing removal organic polluter.
The beneficial effects of the present invention are:
(1) present invention is in ZrCl4And H2Benzoic acid is added in BDC to go to carry out fabricated in situ, adjusts crystal habit, generates
UiO-66-B, then chloroform activation, obtain UiO-66-BA material, mode through the invention is that finally obtained material morphology is
Vertical octahedral structure, has many advantages, such as absorption property height, and stability is good；
(2) benzoic acid, which is adjusted, has synergistic effect between chloroform activation, and zero defect structure can be just obtained after collaboration
UiO-66-BA material, and preparation process is simple, and raw materials are cheap and easy to get, it is at low cost, meet environmental-friendly requirement.
And the method for the present invention does not need the pre-treatment of high temperature, calcining etc, to reduce energy consumption and reaction cost, preparation is simple,
Convenient for batch production.
Detailed description of the invention
The XRD spectrum of Fig. 1 UiO-66, UiO-66-A, UiO-66-B and UiO-66-BA material.
The FTIR map of Fig. 2 UiO-66, UiO-66-A, UiO-66-B and UiO-66-BA material.
The N of Fig. 3 UiO-66, UiO-66-A, UiO-66-B and UiO-66-BA material2Adsorption/desorption figure.
The SEM image of Fig. 4 UiO-66-BA material.
(illustration is the derivative of TGA to the TGA image of Fig. 5 UiO-66, UiO-66-A, UiO-66-B and UiO-66-BA material
Curve).
Fig. 6 UiO-66, UiO-66-A, UiO-66-B and UiO-66-BA material is to the figure of Congo red removal rate, and (5mg inhales
Attached dose；50ml initial concentration is the Congo red solution of 50mg/l).
Fig. 7 is the SEM image of UiO-66-B material made from comparative example 1.
Fig. 8 is the SEM image of UiO-66-A material made from comparative example 2.
Specific embodiment:
The following describes the present invention in detail with reference to examples, so that those skilled in the art more fully understand this hair
It is bright, but the invention is not limited to following embodiments.
Embodiment 1:
UiO-66-BA passes through solvent structure.Specifically carry out as follows:
(1) by 0.386g (1.67mmol) ZrCl4, 0.276g (1.67mmol) H2BDC and 6.118g (50.1mmol) benzene first
Acid dissolution is poured into the stainless steel autoclave equipped with polytetrafluoroethyllining lining after mixing evenly in 50ml DMF solution.
Wherein ZrCl4: H2BDC: the molar ratio of benzoic acid is 1:1:30.
(2) then reaction kettle is placed in air dry oven and is heated 24 hours with 120 DEG C.After reaction kettle is cooled to room temperature
Centrifugation obtains white crystal.
(3) obtained white crystal is washed with DMF and methanol and is immersed in 100ml methanol solution and in reaction kettle afterwards three times
In 100 DEG C handle 12 hours, filtered after processing, wash filter cake, drying, obtain powder.
(4) above-mentioned powder is immersed in chloroform 5 days, filters, obtains sample and be centrifuged with methanol, collected lower sediment, finally exist
In vacuum drying oven 100 DEG C drying 12 hours to obtain UiO-66-BA.
Prepared UiO-66-BA material is after adsorbing Congo red solution 3h to Congo red adsorption rate up to 93.6%.
Comparative example 1
Prepare UiO-66-B: the preparation method of UiO-66 (UiO-66-B) material that benzoic acid is adjusted, comprising the following steps:
(1) by 0.386g (1.67mmol) ZrCl4, 0.276g (1.67mmol) H2BDC and 6.118g (50.1mmol) benzene first
Acid dissolution is poured into the stainless steel autoclave equipped with polytetrafluoroethyllining lining after mixing evenly in 50ml DMF solution.
Wherein ZrCl4: H2BDC: the molar ratio of benzoic acid is 1:1:30；
(2) then reaction kettle is placed in air dry oven and is heated 24 hours with 120 DEG C, after reaction kettle is cooled to room temperature
Centrifugation obtains white crystal；
(3) then obtained white crystal is washed with DMF and methanol and is immersed in 100ml methanol solution and anti-afterwards three times
Answer in kettle 100 DEG C to handle 12 hours, filtered after processing, wash filter cake, finally in vacuum drying oven 100 DEG C drying 12 hours to obtain
Obtain the UiO-66 material (UiO-66-B) adjusted based on benzoic acid.
Comparative example 2
Prepare UiO-66-A: the preparation method of UiO-66 (UiO-66-A) material of chloroform activation, comprising the following steps:
(1) by 0.386g (1.67mmol) ZrCl4With 0.276g (1.67mmol) H2BDC is dissolved in 50ml DMF solution,
It is poured into the stainless steel autoclave equipped with polytetrafluoroethyllining lining after mixing evenly.Wherein ZrCl4: H2The molar ratio of BDC is
1:1。
(2) then reaction kettle is placed in air dry oven and is heated 24 hours with 120 DEG C, after reaction kettle is cooled to room temperature
Centrifugation obtains white crystal.
(3) obtained white crystal is washed with DMF and methanol and is immersed in 100ml methanol solution and in reaction kettle afterwards three times
In 100 DEG C handle 12 hours.
(4) above-mentioned powder is immersed in chloroform 5 days.Then sample is centrifuged with methanol, finally 100 DEG C in vacuum drying oven
Dry 12 hours to obtain UiO-66-A.
The present invention is by above-mentioned UiO-66-BA, UiO-66-B, UiO-66-A material being prepared to containing congo red
The absorption property of waste water is studied.
Absorption property evaluation: adsorption test carries out in constant temperature water bath oscillation case.5mg adsorbent is added to the 50ml the Congo
In red (50-200mg/l) aqueous solution, and the conical flask equipped with mixture is put into constant temperature water bath oscillation case.The mixing is molten
Liquid vibrates 3 hours in constant temperature water bath oscillation case to reach adsorption equilibrium.Timing takes the Congo red solution of 3ml simultaneously from solution upper surface
Adsorbent in the centrifuge separation removal Congo red solution of 3ml.Using ultraviolet-uisible spectrophotometer (2550, Japanese Shimadzu) most
Congo red absorbance is measured at big wavelength 498nm.Absorbance measurement is carried out to the Congo red solution of various concentration, draws standard
Curve.Congo red concentration is calculated according to the absorbance detected, is denoted as Ct.Initial concentration 50-200mg/l is denoted as C0。
Test results are shown in figure 6 for this: from fig. 6 it can be seen that the rate of adsorption of UiO-66-BA and UiO-66-B is most
Very fast in first 30 minutes, Congo red removal rate is respectively 81.1% and 69.1%, and the suction of UiO-66 and UiO-66-A
Attached much lower velocity, respectively 11.5% and 12.8%.After 120 minutes, adsorption curve has almost no change, and is adsorbed on 180 points
Reach balance in clock.
UiO-66-BA reaches 93.6% to Congo red adsorption rate, and the adsorption rate of UiO-66 is only 15.4%, UiO-
The adsorption rate of 66-B 79%, UiO-66-A adsorption rate 15%.As can be seen that benzoic acid is adjusted and chloroform activates to obtain
UiO-66-BA substantially increase to Congo red absorption property.From the point of view of mechanism of mass transfer, at absorption initial stage, when with absorption
Between extension, the Congo red rate of adsorption to UiO-66-BA increases sharply.At this point, Congo red absorption may occur mainly in
On the surface of UiO-66-BA and the outer surface in hole.In the absorption later period, absorption is controlled by diffusion, and diffusion is likely to occur in channel
Surface, therefore the rate of adsorption slows down.After 180 minutes, absorption reaches equilibrium stage.Picture in Fig. 6, which is shown, to be added accordingly
Adsorbent after Congo red solution decoloration.
And adsorbing congo red (CR) experiment shows the UiO-66-BA material for adding benzoic acid and chloroform with non-
Normal efficient absorption property, maximal absorptive capacity 1371mg/g, be under the same terms unmodified UiO-66 to the 7 of CR adsorbance
Times.
UiO- prepared by UiO-66-B prepared by UiO-66-BA that embodiment 1 is prepared, comparative example 1, comparative example 2
66-A and UiO-66 is by X-ray diffraction (XRD), the infrared figure of Fourier (FTIR), scanning electron microscope (SEM), N2Absorption is de-
Fufen analyses (BET) and thermogravimetric analysis (TGA) to prove.
Fig. 1 is UiO-66, UiO-66-A, the XRD spectrum of UiO-66-B and UiO-66-BA material.As can be seen from Fig., exist
Very wide peak (the 2 θ ranges across 2 ° -7 °) are observed in the PXRD figure of UiO-66-B.This " broad peak " is considered by we
Very small " nanosection " of the missing cluster defect promoted is adjusted by monocarboxylic acid.However, not having in the mode of UiO-66-BA
See this " broad peak ".This phenomenon is to make its knot since activation process can be reduced unreacted benzene dicarboxylic acid connector
To obtain zero defect structure in structure.In addition, the synergistic effect between benzoic acid and chloroform activation promotes according to the intensity of diffraction maximum
The formation of high-crystallinity UiO-66.
XRD spectrum illustrates that the UiO-66-BA of preparation has the diffraction maximum being remarkably reinforced, to illustrate that UiO-66-BA has
Better crystallinity.
Fig. 2 is UiO-66, UiO-66-A, the FTIR map of UiO-66-B and UiO-66-BA material.For UiO-66, wave
Number is 3423cm-1,1574cm-1(1401cm-1) and 1506cm-1Absorption peak represent the OH group of outer surface, O- in BDC ligand
Asymmetric stretch of C-O is respectively present in the C=C of phenyl ring with typical vibration.In addition, 664 and 748cm-1The peak attribution at place
In the μ of Zr- (OC)3- O stretching, extension.These peaks on UiO-66 appear on other three kinds of materials, show these materials and UiO-66
Similitude.However, having a noticeable place is wave number occur on UiO-66-B and UiO-66-BA to be
1708cm-1Weak peak, indicate benzoic acid in C=O stretching vibration.This may be due to being added to benzoic acid.
Fig. 3 is UiO-66, UiO-66-A, the N of UiO-66-B and UiO-66-BA material2Adsorption/desorption figure.All samples
The nitrogen absorption measurement that porosity and surface area pass through 77K.The surface area of UiO-66 sample is 750m2/g.However, living with chloroform
It after change, potentially contributes to obtain the UiO-66 of more perfect structure without unreacted BDC, increases specific surface area and aperture.In addition,
The specific surface area of UiO-66 and aperture increase with the addition of benzoic acid.N2The ratio of adsorption/desorption analytic explanation UiO-66-BA
The UiO-66 of surface area, microporosity, porosity and aperture compared to unused benzoic acid and/or chloroform is increased considerably.
Fig. 4 is the SEM image of UiO-66-BA material.UiO-66-BA, which has, as can be observed from Figure founds octahedral nothing
Defect sturcture.
Fig. 5 is UiO-66, UiO-66-A, the TGA image of UiO-66-B and UiO-66-BA material.UiO-66 and its derivative
The weight loss of nanocrystal substantially occurs at the same temperature, shows the thermal stability of skeleton not by the addition and activation of acid
Influence.
It is found that there is association between after the adjustment effect of benzoic acid and chloroform activation are combined after comparative analysis in above-mentioned figure
Same-action.After the activation of UiO-66-B material chloroform, the property such as the structure and specific surface of the UiO-66-BA made, adsorptivity
It can make moderate progress.
The embodiment is a preferred embodiment of the present invention, but present invention is not limited to the embodiments described above, not
In the case where substantive content of the invention, any conspicuous improvement that those skilled in the art can make, replacement
Or modification all belongs to the scope of protection of the present invention.
Claims (4)
1. being adjusted based on benzoic acid and chloroform activating the method for preparing UiO-66, which is characterized in that the preparation method is specific
Step are as follows:
(1) by ZrCl4, H2BDC and benzoic acid are dissolved in DMF, are poured into after mixing evenly equipped with the stainless of polytetrafluoroethyllining lining
In steel autoclave；
(2) then reaction kettle is placed in air dry oven and is heated 24 hours under the conditions of 120 DEG C, is cooled to room temperature to reaction kettle
Centrifugation obtains white crystal afterwards；
(3) obtained white crystal is washed with DMF and methanol respectively, the crystal after washing, which immerses in methanol solution, to be placed in instead
It answers in kettle, handles 12 hours under the conditions of 100 DEG C, filtered after processing, collect filter cake and wash, dry, obtain powder；
(4) above-mentioned powder is immersed in chloroform 5 days, filters, obtains sample and be centrifuged with methanol, lower sediment is collected, in vacuum drying oven
Middle drying obtains the UiO-66 material (UiO-66-BA) adjusted based on benzoic acid with chloroform activation.
2. the method according to claim 1 adjusted based on benzoic acid and chloroform activation prepares UiO-66, it is characterised in that:
The ZrCl4: H2BDC: the molar ratio of benzoic acid is 1:1:30.
3. the method according to claim 1 adjusted based on benzoic acid and chloroform activation prepares UiO-66, it is characterised in that:
Drying condition described in step (4) are as follows: 12 hours dry at 100 DEG C.
4. the UiO-66's that method preparation according to claim 1-3 is adjusted based on benzoic acid and chloroform activates answers
With, which is characterized in that the UiO-66 material is as adsorbent for removing removal organic polluter.
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| CN111545171A (en) * | 2020-04-16 | 2020-08-18 | 南昌航空大学 | Preparation method of acid-resistant Zr-MOF material for selectively adsorbing hexavalent chromium |
| CN113307982A (en) * | 2021-06-24 | 2021-08-27 | 河南中医药大学 | Preparation method and application of Cd/Zr-UIO-66 bimetallic organic framework material |
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Application publication date: 20190409 |