CN105642238B - A kind of SiO2The preparation method and application of@MIL-68 (Al) composite material - Google Patents
A kind of SiO2The preparation method and application of@MIL-68 (Al) composite material Download PDFInfo
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- CN105642238B CN105642238B CN201610109719.8A CN201610109719A CN105642238B CN 105642238 B CN105642238 B CN 105642238B CN 201610109719 A CN201610109719 A CN 201610109719A CN 105642238 B CN105642238 B CN 105642238B
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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
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
- C02F2101/00—Nature of the contaminant
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Abstract
A kind of SiO2The preparation method and application of@MIL 68 (Al) composite material, by SiO2It is distributed in DMF, then adds in BDC, AlCl3·6H2O and DMF carries out that final product is obtained by the reaction.Pass through composite S iO2Into MIL 68 (Al), the particle size of MIL 68 (Al) becomes smaller, is distributed change uniformly, and pore size becomes smaller.This composite material can reach the aniline in aqueous solution removing rapidly and efficiently.
Description
Technical field
The present invention relates to the preparation and application of silica and metal-organic framework composite material, and in particular to a kind of
The better SiO of particle size smaller dispersiveness2The preparation of@MIL-68 (Al) composite material, for the quick, high of aniline in aqueous solution
Effect removing.
Background technology
Metal-organic framework (Metal-Organic Frameworks, MOFs) material is mainly by oxygen-containing or nitrogen
The organic ligand multidimensional periodicity mesh skeleton that is connected and is formed with transition metal ions.Big Chang Yinqi specific surface area, height
Porosity, structure and functional group's adjustability be widely used in the necks such as adsorbing separation, catalysis, sensing, electrochemistry, biomedicine
Domain.But simultaneously because its stability is poor, production cost height etc. is limited in laboratory, can not industrialized production use.
MIL-68 (Al) preparation method is simple, raw material is cheap, and cost of manufacture is cheaply many compared with other MOFs, chemical stability
And better heat stability, haveAndTwo kinds of holes, in pollutant adsorbing and removing and gas absorption separation side
There is potential application in face.Nano-meter SiO_22It is very often because the Si-O-H groups on its surface can provide nucleation position for the growth of MOFs
Basis material.
Aniline as a kind of very cheap chemical industry chemicals, is widely used in petrochemical industry and produces, bio-pharmaceuticals,
Rubber, polymer, Insecticides (tech) ＆ Herbicides (tech), dyestuff, pigment production in.However, aniline is high poison again, it can be to life after contact
Object can cause serious injury, if people contacts aniline, may obtain hemolytic anemia, liver kidney be caused to damage, even
Stupor property shock.According to reported in literature, the aniline being discharged into every year in environment is up to 30,000 tons, so being carried out to aniline waste water large quantities of
The processing of amount has been very urgent.For this problem, we are prepared one kind and can be used with repeated regeneration, and in 20s i.e.
The adsorbent of efficient absorption can be reached --- SiO2@MIL-68 (Al) composite material, which, which has, is more suitable for aniline absorption
Micropore, cost of manufacture is not high, is suitble to extensive reuse.
The content of the invention
The purpose of the present invention is be directed to the analysis of above-mentioned technology and there are the problem of, a kind of SiO is provided2@MOF composite materials
Preparation method and applications, the preparation method dexterously utilize Nano-meter SiO_22The silicone hydroxyl on surface can be for MIL-68's (Al)
Synthesis provides the fact that nucleation position, to Nano-meter SiO_22Microsphere surface uniformly coats, and effectively avoids MIL-68 (Al) particle
Size Distribution is uneven, Nano-meter SiO_22The problem of easily reuniting, preparation method is simple and easy to do.The composite material is used for aqueous solution
A kind of method of efficient fast eliminating phenol is established in the removing of middle aniline.
A kind of SiO2The preparation method of@MIL-68 (Al) composite material, comprises the following steps：
(1) by SiO2It is added to N, in N '-dimethyl formamide (DMF), ultrasonic disperse forms SiO2DMF suspensions；
(2) by terephthalic acid (TPA) (BDC) and Aluminium chloride hexahydrate (AlCl3·6H2O) it is added in above-mentioned suspension, ultrasound
Rotor is added in simultaneously, after 10h is stirred at room temperature, is persistently stirred under the conditions of 130 DEG C, after reacting 18.5h, is cooled to room temperature, is filtered,
Obtain product；
(3) by obtained product successively with N, N '-dimethyl formamide, methanol cleaning, then under vacuum degree condition
Heat drying obtains SiO2@MIL-68 (Al) composite material.
Reactant SiO in building-up process2:BDC:AlCl3·6H2O:N, the molar ratio of N '-dimethyl formamide is (2.5-
12.5):30:20:3891, preferably 7.49:30:20:3891.
The SiO of above-mentioned preparation2@MIL-68 (Al) composite material is used for the removing of aniline in aqueous solution.
Beneficial effects of the present invention are：Pass through the SiO of one-step synthesis method2@MIL-68 (Al) composite material, particle size are small
And uniformly, pore size distribution is uniform.This material can be in efficiently quick adsorption aqueous solution aniline.The SiO2@MIL-68
(Al) preparation method of composite material, Nano-meter SiO_2 used2Size be about 30-40nm.The particle of composite material is compared with MIL-68
(Al) particle becomes smaller, and distribution becomes uniform.The pore size of composite material becomes smaller compared with the pore size of MIL-68 (Al), and pore size distribution becomes
Uniformly.
Description of the drawings
Fig. 1 is X-ray diffractogram (XRD)：(a)MIL-68(Al)；(b) SiO that embodiment 1 obtains2@MIL-68(Al)；
(c) SiO that embodiment 2 obtains2@MIL-68(Al)。
Fig. 2 is electron scanning micrograph (SEM)：(a)MIL-68(Al)；(b) SiO that embodiment 1 obtains2@MIL-
68(Al)；(c) SiO that embodiment 2 obtains2@MIL-68(Al)； (d)SiO2。
Fig. 3 is accumulation pore volume distribution：(a)MIL-68(Al)；(b) SiO that embodiment 2 obtains2@MIL-68(Al)。
Fig. 4 is the SiO that (a) embodiment 2 obtains at 25 DEG C2@MIL-68 (Al) and (b) MIL-68 (Al) are to 1000ppm
Aniline solution the curve that changes over time of adsorbance.
Fig. 5 is the SiO that (a) embodiment 2 obtains at 25 DEG C2The SiO that@MIL-68 (Al) and (b) embodiment 1 obtain2@MIL-
68 (Al) are to the adsorption isotherm of aniline.
Specific embodiment
With reference to the accompanying drawings and examples, the present invention is further elaborated, but the present invention is not limited thereto.
Comparative example 1
By 5g terephthalic acid (TPA)s (BDC), 4.88g Aluminium chloride hexahydrates (AlCl3·6H2O) it is added to 300mL DMF
In 500mL round-bottomed flasks, rotor is added in, is persistently stirred under the conditions of 130 DEG C, after reacting 18.5h, be cooled to room temperature, filtered, obtain
To product, obtained product is cleaned three times successively with 50mL DMF, 50mL methanol cleans four times, then in vacuum degree
The dry 10h of lower 150 DEG C of 0.1MPa, obtain MIL-68 (Al) material.
Embodiment 1
SiO2The preparation of@MIL-68 (Al) composite material, by 0.24g SiO2500mL round bottoms are added to 300mL DMF to burn
In bottle, ultrasonic disperse 30min forms SiO2DMF suspensions.By six chloride hydrate of 5g terephthalic acid (TPA)s (BDC) and 4.88g
Aluminium (AlCl3·6H2O) it is added in above-mentioned suspension, ultrasonic 10min, rotor is added in, after 10h is stirred at room temperature, in 130 DEG C of items
It persistently stirs under part, after reacting 18.5h, is cooled to room temperature, filter, obtain product, obtained product is used into 50mL successively
DMF is cleaned three times, and 50mL methanol cleans four times, and then 150 DEG C of dry 10h under vacuum degree 0.1MPa, obtain SiO2@MIL-68
(Al) composite material.
Embodiment 2
SiO2The preparation of@MIL-68 (Al) composite material, by 0.45g SiO2500mL round bottoms are added to 300mL DMF to burn
In bottle, ultrasonic disperse 30min forms SiO2DMF suspensions.By 5g terephthalic acid (TPA)s (BDC) and 4.88g Aluminium chloride hexahydrates
(AlCl3·6H2O) it is added in above-mentioned suspension, ultrasonic 10min, rotor is added in, after 10h is stirred at room temperature, under the conditions of 130 DEG C
Lasting stirring, after reacting 18.5h, is cooled to room temperature, and filters, obtains product, and obtained product is clear with 50mL DMF successively
It washes three times, 50mL methanol cleans four times, and then 150 DEG C of dry 10h under vacuum degree 0.1MPa, obtain SiO2@MIL-68(Al)
Composite material.
Embodiment 3
The SiO prepared using embodiment 1, embodiment 22@MIL-68 (Al) carry out the removing of aniline in aqueous solution.
First, the aqueous solution of the aniline of certain initial concentration is prepared, 10mL is taken to add in being threaded in the bottle of plastic lid
Enter 10mg SiO2@MIL-68 (Al) composite material, whole system, which is placed in 25 DEG C of constant-temperature tables, shakes 2h, followed by 0.22
μm polyethersulfone filter filtering obtain clear liquid, after dilution using ultraviolet-uisible spectrophotometer test solution at 230nm
Peak value obtains respective concentration, and is compared with the concentration of initial soln, obtains at 25 DEG C material to the adsorption isotherm of aniline
Line, then acquired results are carried out with Langmuir simulations, SiO is calculated2@MIL-68 (Al) composite material (especially embodiment 2)
537.6mg/g is up to the maximal absorptive capacity of aniline.
Embodiment 4
The SiO prepared using embodiment 22@MIL-68 (Al) carry out the dynamics research and again of aniline in aqueous solution absorption
Raw performance study.
First, the aqueous solution of the aniline of 1000mg/L initial concentrations is prepared, takes 10mL in the bottle for being threaded plastic lid
In, add in 10mg SiO2@MIL-68 (Al) composite material, whole system, which is placed in shaking table, shakes the different time, followed by
0.22 μm of polyethersulfone filter filtering obtains clear liquid, and solution is tested in 230nm using ultraviolet-uisible spectrophotometer after dilution
The peak value at place obtains respective concentration, and is compared with the concentration of initial soln.The study found that SiO2@MIL-68 (Al) are multiple
Condensation material reaches adsorption saturation to the absorption of aniline in 20s.Finally, we are to completing the SiO after adsorbing2@MIL-68
(Al) composite material is regenerated, and the method for use is that methanol is added in the material after filtering, is ultrasonically treated 30min, then
The lower 150 DEG C of freeze-day with constant temperature 10h of vacuum degree 0.1MPa are reused for the adsorbing and removing of aniline, which repeats five times, and regenerate every time
Afterwards, adsorbance does not significantly decrease.
After materials synthesis, the compound front and rear material is characterized and performance detection.
Fig. 1 compares for X-ray diffractogram (XRD).It can be seen that compound front and rear, the diffraction maximum of MIL-68 (Al) powder
That matches somebody with somebody is very good, illustrates SiO2Introducing do not change MIL-68 (Al) structure of itself.
Fig. 2 is the electron scanning micrograph (SEM) of material, and wherein a figure MIL-68 (Al), b, c figures are SiO2@
MIL-68 (Al), d figures are SiO2.It can be seen that SiO2Introducing the particle size of MIL-68 (Al) is made to become smaller, particle dispersion
Improve.
Fig. 3 is the accumulation pore volume distribution comparison diagram of compound front and rear material, and wherein a figure MIL-68 (Al), b figures are SiO2@
MIL-68(Al).It can be seen that SiO2@MIL-68 (Al) are more concentrated than MIL-68 (Al) hole smaller, distribution, are had a large amount of small
InMicropore, being more suitable for size isAniline absorption.
Fig. 4 is (a) SiO2@MIL-68 (Al) and (b) MIL-68 (Al) to the adsorbance of the aniline solution of 1000ppm at any time
Between the curve that changes.As can be seen that MIL-68 (Al) just reaches adsorption equilibrium in 30min, and SiO2@MIL-68 (Al) exist
Reach adsorption equilibrium when 20s.
Fig. 5 is the SiO of two doping ratios at 25 DEG C2@MIL-68 (Al) composite materials lead to the adsorption isotherm of aniline
It crosses Langmuir simulations and maximal absorptive capacity is calculated as 537.6 mg/g.
The present invention is not limited to above-mentioned preferred forms, anyone can show that other are various under the enlightenment of the present invention
The product of form, however, make any variation in its shape or structure, it is every that there is skill identical or similar to the present application
Art scheme, within the protection domain for all falling within patent of the present invention.
Claims (5)
1. a kind of quick, efficient removal SiO for aniline in aqueous solution2The preparation method of@MIL-68 (Al) composite material,
It is characterised in that it includes following steps：
(1) by SiO2It is added to N, in N '-dimethyl formamide (DMF), ultrasonic disperse forms SiO2DMF suspensions；
(2) by terephthalic acid (TPA) (BDC) and Aluminium chloride hexahydrate (AlCl3·6H2O) it is added in above-mentioned suspension, ultrasound is simultaneously
Rotor is added in, after 10h is stirred at room temperature, is persistently stirred under the conditions of 130 DEG C, after reacting 18.5h, is cooled to room temperature, filters, obtains
Product；
(3) by obtained product successively with N, then N '-dimethyl formamide, methanol cleaning are heated under vacuum degree condition
It is dry, obtain SiO2@MIL-68 (Al) composite material；
SiO2Size be 30-40nm.
2. according to the SiO of claim 12The preparation method of@MIL-68 (Al) composite material, which is characterized in that anti-in building-up process
Answer object SiO2:BDC:AlCl3·6H2O:N, the molar ratio of N '-dimethyl formamide is (2.5-12.5):30:20:3891.
3. according to the SiO of claim 12The preparation method of@MIL-68 (Al) composite material, which is characterized in that SiO2:BDC:
AlCl3·6H2O:N, the molar ratio of N '-dimethyl formamide is 7.49:30:20:3891.
4. the SiO prepared according to any one of claim 1-3 the method2@MIL-68 (Al) composite material.
5. the SiO prepared according to any one of claim 1-3 the method2The application of@MIL-68 (Al) composite material, for water
The removing of aniline in solution.
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| CN110694589B (en) * | 2019-09-30 | 2022-04-05 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Metal organic framework-silicon-based composite material and preparation method and application thereof |
| CN112054178A (en) * | 2020-09-14 | 2020-12-08 | 大连理工大学 | Porous silicon @ silicon oxide @ Al-MOF negative electrode material for lithium ion battery and preparation method and application thereof |
| CN114085539B (en) * | 2021-12-07 | 2023-03-31 | 万华化学（宁波）有限公司 | Super-hydrophobic low-precipitation degradable material and preparation method thereof |
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| CN102249363A (en) * | 2011-07-13 | 2011-11-23 | 北京化工大学 | Method for using metal-organic framework material to purify water, exchange ions with water or magnetize water |
| CN103521269A (en) * | 2013-11-04 | 2014-01-22 | 北京化工大学 | Metal-organic framework materials with magnetic cores and preparation and application thereof |
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| CN105056895A (en) * | 2015-08-17 | 2015-11-18 | 中国科学院上海高等研究院 | Preparation method and application of metal organic frameworks-mesoporous silica composite material |
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| KR101663184B1 (en) * | 2009-12-15 | 2016-10-06 | 삼성전자주식회사 | Hybrid porous material and method of preparing same |
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| CN102249363A (en) * | 2011-07-13 | 2011-11-23 | 北京化工大学 | Method for using metal-organic framework material to purify water, exchange ions with water or magnetize water |
| CN103521269A (en) * | 2013-11-04 | 2014-01-22 | 北京化工大学 | Metal-organic framework materials with magnetic cores and preparation and application thereof |
| CN103551196A (en) * | 2013-11-11 | 2014-02-05 | 北京化工大学 | Magnetic metal-organic framework material with mesoporous structure and preparation and catalysis reaction thereof |
| CN105056895A (en) * | 2015-08-17 | 2015-11-18 | 中国科学院上海高等研究院 | Preparation method and application of metal organic frameworks-mesoporous silica composite material |
Non-Patent Citations (1)
| Title |
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| "Synthesis of CNT@MIL-68(Al) composites with improved adsorption capacity for phenol in aqueous solution";Tongtong Han et al.,;《Chemical Engineering Journal》;20150408;第275卷;第134页摘要、第135页2.4 CNT@MIL-68(Al)复合材料的合成，2.3 MIL-68(Al)的合成，第139页 4.总结 * |
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