CN107376852A - A kind of preparation method of@FP composite adsorbing materials of HKUST 1 and its application in adsorption cleaning handles lead waste water - Google Patents
A kind of preparation method of@FP composite adsorbing materials of HKUST 1 and its application in adsorption cleaning handles lead waste water Download PDFInfo
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- CN107376852A CN107376852A CN201710762533.7A CN201710762533A CN107376852A CN 107376852 A CN107376852 A CN 107376852A CN 201710762533 A CN201710762533 A CN 201710762533A CN 107376852 A CN107376852 A CN 107376852A
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3433—Regenerating or reactivating of sorbents or filter aids other than those covered by B01J20/3408 - B01J20/3425
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
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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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- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
Application the invention discloses a kind of preparation method of@FP composite adsorbing materials of HKUST 1 and its in adsorption cleaning handles lead waste water, first by 3.114g Cu (NO3)·3H2O, which is dissolved in 22.5mL deionized waters, obtains solution A, by the benzenetricarboxylic acid ultrasonic dissolutions of 1.5g 1,3,5 in 45mL volume ratios be 1:1 absolute ethyl alcohol and N, solution B is obtained in the mixed solution of N dimethylformamides, solution A and solution B are mixed, and 4cm × 4cm filter paper is added in above-mentioned mixed system, transfer in polytetrafluoroethyllining lining reactor and react 12h in 90 DEG C, take out filter paper after the completion of reaction, rinsed repeatedly with deionized water, finally dry and composite adsorbing material is made, and specifically disclose application of the obtained composite adsorbing material in adsorption cleaning handles lead waste water.Preparation process technique of the present invention is simple and condition is controllable, obtained composite adsorbing material can selectively from waste water adsorpting lead ion, adsorbed again with 0.2mol/L thiourea solution desorption after absorption, after 5 times recycle, composite adsorbing material still has higher absorption property to lead.
Description
Technical field
Adsorption cleaning processing technology field the invention belongs to the synthesis of composite adsorbing material and its for lead waste water, tool
Body is related to a kind of preparation method of HKUST-1@FP composite adsorbing materials and its application in adsorption cleaning handles lead waste water.
Background technology
HKUST-1 chemical formula is:Cu3(C9H3O6)2, as a member in metal-organic framework materials, by Hong Kong science and technology
The Williams professors of university synthesized first in 1999.In gas storage, biomedicine, magnetic composite, catalysis
Show good application prospect with fields such as fluorescence.
Filter paper(Filter Paper, FP)The filtering material common as laboratory, there are some excellent characteristics:(1)
It is cheap, it is readily obtained;(2)It is biodegradable, it is easily handled;(3)Good mechanical property;(4)The inside of filter paper has countless
Aperture, play a part of capillary;(5)The cellulose of composition filter paper has substantial amounts of hydroxy functional group, these high activities
A variety of chemical reactions can occur for hydroxyl.Therefore, filter paper is the good carrier for preparing functional composite material.
The content of the invention
Present invention solves the technical problem that there is provided a kind of HKUST-1@FP composite adsorbing materials preparation method and its
HKUST-1 is loaded on filter paper and is successfully prepared HKUST-1@FP by the application in adsorption cleaning handles lead waste water, this method
Composite adsorbing material, the lead that the HKUST-1@FP composite adsorbing materials can be used in selective absorption waste water, and after regeneration
Being capable of repetitive cycling use.
The present invention is to solve above-mentioned technical problem to adopt the following technical scheme that, a kind of HKUST-1@FP composite adsorbing materials
Preparation method, it is characterised in that concretely comprise the following steps:First by 3.114g Cu (NO3)·3H2O, which is dissolved in 22.5mL deionized waters, to be obtained
To solution A, by the benzenetricarboxylic acid ultrasonic dissolutions of 1.5g 1,3,5- in 45mL volume ratios be 1:1 absolute ethyl alcohol and N, N- dimethyl
Solution B is obtained in the mixed solution of formamide, solution A and solution B are mixed, and 4cm × 4cm filter paper is added to above-mentioned mix
In zoarium system, transfer in polytetrafluoroethyllining lining reactor and react 12h in 90 DEG C, take out filter paper after the completion of reaction, spend
Ionized water rinses repeatedly, finally dries and HKUST-1@FP composite adsorbing materials are made.
Application of the HKUST-1@FP composite adsorbing materials of the present invention in adsorption cleaning handles lead waste water, it is special
Sign is that detailed process is:Adsorption process, HKUST-1@FP composite adsorbing materials are added in lead waste water, in 30 DEG C of absorption
300min realizes the adsorption cleaning processing of lead waste water;Desorption process, the HKUST-1@FP composite adsorbing materials after absorption are added
Enter in the thiourea solution for being 0.2mol/L to molar concentration, after vibration desorption 24h, take out HKUST-1@FP composite adsorbing materials warp
Repetitive cycling uses after deionized water rinsing.
Preparation process technique of the present invention is simple and condition is controllable, and obtained HKUST-1@FP composite adsorbing materials can select
Property from waste water Adsorption of Lead, thiourea solution that the composite adsorbing material after absorption is 0.2mol/L with molar concentration desorption inhales again
Attached, after 5 times recycle, HKUST-1@FP composite adsorbing materials still have higher absorption property to lead.
Brief description of the drawings
Fig. 1 is FP, HKUST-1 and HKUST-1@FP infrared spectrum;
Fig. 2 is FP, HKUST-1 and HKUST-1@FP XRD spectra;
Fig. 3 is FP SEM figures;
Fig. 4 is HKUST-1 SEM figures;
Fig. 5 is HKUST-1@FP SEM figures;
Fig. 6 is the kinetic curve of HKUST-1@FP Adsorption of Lead;
Fig. 7 is influence curve of the initial concentration to lead clearance;
Fig. 8 is influence curves of the pH to lead adsorption.
Embodiment
The above of the present invention is described in further details by the following examples, but this should not be interpreted as to this
The scope for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair
Bright scope.
Embodiment 1
1st, the preparation of HKUST-1@FP composite adsorbing materials:
First by 3.114g Cu (NO3)·3H2O, which is dissolved in 22.5mL deionized waters, obtains solution A, by the benzene three of 1.5g 1,3,5-
Formic acid ultrasonic dissolution is 1 in 45mL volume ratios:Solution is obtained in 1 absolute ethyl alcohol and the mixed solution of N,N-dimethylformamide
B, solution A and solution B are mixed, and 4cm × 4cm filter paper is added in above-mentioned mixed system, be then transferred to polytetrafluoroethyl-ne
12h is reacted in 90 DEG C in alkene liner reactor, filter paper is taken out after the completion of reaction, is rushed repeatedly with deionized water, finally drying is made
HKUST-1@FP composite adsorbing materials.
2nd, characterize:
Fig. 1 is FP, HKUST-1 and HKUST-1@FP infrared spectrum.As seen from the figure, the characteristic peak of the oh group on filter paper exists
3404cm-1Place, 2899cm-1What place represented is C-H stretching vibration.HKUST-1 infrared spectrum is in 1645cm-1The feature at place
What peak represented is the asymmetric stretching vibration of the carbonyl group of part carboxylic acid.And HKUST-1@FP characteristic peak had both contained filter
The characteristic peak of paper also contains HKUST-1 characteristic peak, illustrates that HKUST-1 successes are immobilized and has arrived on filter paper.
Fig. 2 is FP, HKUST-1 and HKUST-1@FP XRD spectra.HKUST-1@FP XRD spectra occur with
HKUST-1 corresponds to consistent characteristic diffraction peak, while consistent characteristic diffraction peak corresponding with filter paper, this explanation also occurs
HKUST-1 is successfully loaded on filter paper, prepares [email protected] crystal structure is not destroyed.
Fig. 3-5 is FP, HKUST-1 and HKUST-1@FP scanning electron microscope (SEM) photograph respectively.The shape characteristic significant difference of three.
Filter paper fibre is high-visible, and HKUST-1 is into bulk, and HKUST-1 FP surfaces are not it is observed that filter paper fibre, block
HKUST-1 is high-visible, and this explanation HKUST-1 is successfully loaded on filter paper.
3rd, absorption property:
Fig. 6 is the kinetic curve of HKUST-1@FP Adsorption of Lead.The adsorbent is fast to the adsorption rate of lead, and experiment condition is:Lead
Initial concentration is respectively 200mg/L and 100mg/L, volume 50mL, HKUST-1@FP composite adsorbing material 200mg, temperature 30
DEG C, oscillation rate 160rpm.
Fig. 7 is influence curve of the initial concentration to lead clearance.In the range of wider initial concentration, lead clearance reaches
More than 96%, experiment condition is:Volume is 50mL, HKUST-1@FP composite adsorbing material 200mg, 30 DEG C of temperature, oscillation rate
160rpm, time 300min.
Fig. 8 is influence curves of the pH to lead adsorption.Experiment condition is:Lead initial concentration is 200mg/L, and volume is
50mL, HKUST-1@FP composite adsorbing material 200mg, 30 DEG C, oscillation rate 160rpm, time 300min of temperature.
Table 1 is influence of other coexistent metallic ions to HKUST-1@FP Adsorption of Lead.As seen from table:In common metal ion
Under conditions of coexisting, HKUST-1@FP remain to effectively adsorb to lead.Experiment condition is:Lead initial concentration is 200mg/L, other common
It is 50mg/L to deposit concentration of metal ions, volume 50mL, HKUST-1@FP composite adsorbing material 200mg, 30 DEG C of temperature, is vibrated
Speed 160rpm, time 300min.
Influence of the coexistent metallic ion of table 1 to HKUST-1@FP Adsorption of Lead
The regeneration cycle of HKUST-1@FP composite adsorbing materials uses
HKUST-1@FP after adsorpting lead ion are added in 0.2mol/L thiourea solution, after vibration desorption 24h, taken out
HKUST-1@FP, are then added to through deionized water rinsing in lead ion initial concentration 200mg/L solution, vibration absorption
300min, so repeatedly absorption-elution-sorption cycle 5 times again.HKUST-1@FP are followed successively by the adsorbance of lead:46.9mg/g、
46.2mg/g, 45.1mg/g, 43.6mg/g and 42.7mg/g, this illustrates the HKUST-1@FP composite adsorbing materials through 5 repetitions
Still there is higher adsorption capacity after use to lead.
Claims (2)
1. a kind of preparation method of HKUST-1@FP composite adsorbing materials, it is characterised in that concretely comprise the following steps:First by 3.114g
Cu(NO3)·3H2O, which is dissolved in 22.5mL deionized waters, obtains solution A, by the benzenetricarboxylic acid ultrasonic dissolutions of 1.5g 1,3,5- in 45mL
Volume ratio is 1:Solution B is obtained in 1 absolute ethyl alcohol and the mixed solution of DMF, solution A and solution B are mixed
Close, and 4cm × 4cm filter paper is added in above-mentioned mixed system, transfer in polytetrafluoroethyllining lining reactor in 90
DEG C reaction 12h, takes out filter paper after the completion of reaction, is rinsed repeatedly with deionized water, finally dry and HKUST-1 FP compound suctions are made
Enclosure material.
2. HKUST-1@FP composite adsorbing materials made from the method according to claim 11 are leaded useless in adsorption cleaning processing
Application in water, it is characterised in that detailed process is:Adsorption process, HKUST-1@FP composite adsorbing materials are added to leaded useless
In water, the adsorption cleaning processing that 300min realizes lead waste water is adsorbed in 30 DEG C;Desorption process, by the HKUST-1@FP after absorption
Composite adsorbing material is added in the thiourea solution that molar concentration is 0.2mol/L, after vibration desorption 24h, takes out HKUST-1@FP
Composite adsorbing material repetitive cycling after deionized water rinsing uses.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107880278A (en) * | 2017-12-07 | 2018-04-06 | 宁波诺丁汉新材料研究院有限公司 | A kind of porous level metal-organic framework material HKUST 1 preparation method |
CN108786758A (en) * | 2018-06-08 | 2018-11-13 | 河南师范大学 | A kind of preparation method and applications of HKUST-1@PS compound adsorbents for selective absorption methylene blue |
CN108854995A (en) * | 2018-06-08 | 2018-11-23 | 河南师范大学 | The preparation method and applications of HKUST-1@PMMA composite material of the one kind for adsorbing Pb (II) |
CN110787778A (en) * | 2019-11-01 | 2020-02-14 | 中国工程物理研究院材料研究所 | Modified fiber ball filtering and adsorbing material and preparation method and application thereof |
CN113368839A (en) * | 2021-06-16 | 2021-09-10 | 南京工业大学 | Polyaniline-modified organic metal framework heavy metal adsorbing material and preparation method thereof |
CN115501862A (en) * | 2022-09-20 | 2022-12-23 | 河南大学 | Preparation method of wheat bran/HKUST-1 aerogel in aqueous solution |
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107880278A (en) * | 2017-12-07 | 2018-04-06 | 宁波诺丁汉新材料研究院有限公司 | A kind of porous level metal-organic framework material HKUST 1 preparation method |
CN107880278B (en) * | 2017-12-07 | 2021-01-15 | 宁波诺丁汉新材料研究院有限公司 | Preparation method of porous metal organic framework material HKUST-1 |
CN108786758A (en) * | 2018-06-08 | 2018-11-13 | 河南师范大学 | A kind of preparation method and applications of HKUST-1@PS compound adsorbents for selective absorption methylene blue |
CN108854995A (en) * | 2018-06-08 | 2018-11-23 | 河南师范大学 | The preparation method and applications of HKUST-1@PMMA composite material of the one kind for adsorbing Pb (II) |
CN110787778A (en) * | 2019-11-01 | 2020-02-14 | 中国工程物理研究院材料研究所 | Modified fiber ball filtering and adsorbing material and preparation method and application thereof |
CN113368839A (en) * | 2021-06-16 | 2021-09-10 | 南京工业大学 | Polyaniline-modified organic metal framework heavy metal adsorbing material and preparation method thereof |
CN115501862A (en) * | 2022-09-20 | 2022-12-23 | 河南大学 | Preparation method of wheat bran/HKUST-1 aerogel in aqueous solution |
CN115501862B (en) * | 2022-09-20 | 2023-11-21 | 河南大学 | Preparation method of wheat bran/HKUST-1 aerogel in aqueous solution |
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