CN107486164B - Preparation method of ZIF-8@ FP composite adsorption material and application of adsorption material in adsorption and purification treatment of copper-containing wastewater - Google Patents

Preparation method of ZIF-8@ FP composite adsorption material and application of adsorption material in adsorption and purification treatment of copper-containing wastewater Download PDF

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CN107486164B
CN107486164B CN201710764914.9A CN201710764914A CN107486164B CN 107486164 B CN107486164 B CN 107486164B CN 201710764914 A CN201710764914 A CN 201710764914A CN 107486164 B CN107486164 B CN 107486164B
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zif
filter paper
adsorption
composite
distilled water
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CN107486164A (en
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王治科
朱韵怡
陈海天
叶存玲
范顺利
陈凌云
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Henan Normal University
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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]
    • 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
    • B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • 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
    • 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
    • C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
    • 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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  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The invention discloses a preparation method of a ZIF-8@ FP composite adsorption material and application thereof in adsorption and purification treatment of copper-containing wastewater, wherein filter paper is cut into filter paper strips with the thickness of 1cm by 4cm and placed in a sodium hydroxide solution with the mass concentration of 10%, the filter paper strips are oscillated for 2 hours at the temperature of 30 ℃ and at the speed of 120r/min, then the filter paper strips are washed to be neutral by distilled water, and the filter paper strips are dried at the temperature of 60 ℃ to obtain pretreated filter paper for later use; 1.17g of Zn (NO)3)2·6H2Dissolving O in 8mL of distilled water, adding pretreated filter paper, soaking for 20min, dissolving 22.6g of 2-methylimidazole in 80mL of distilled water, pouring the formed 2-methylimidazole solution into the solution for soaking the filter paper, oscillating for 24h at 30 ℃ and 120r/min, standing for 24h, cleaning by using distilled water, and drying at 60 ℃ to obtain the composite adsorbing material. The preparation method of the composite adsorption material has the advantages of simple process, convenient operation and mild conditions, and the prepared composite adsorption material has strong adsorption selectivity, strong anti-interference capability, high adsorption rate and easy separation.

Description

Preparation method of ZIF-8@ FP composite adsorption material and application of adsorption material in adsorption and purification treatment of copper-containing wastewater
Technical Field
The invention belongs to the technical field of composite adsorbents, and particularly relates to a preparation method of a ZIF-8@ FP composite adsorption material and application thereof in adsorption and purification treatment of copper-containing wastewater.
Background
ZIF-8 is a metal organic framework material, has the advantages of good hydrothermal stability, ultra-large specific surface area, adjustable aperture and the like, also has a revolving door effect of adsorbing macromolecules with the aperture larger than that of the ZIF-8, and has become a research hotspot in the field of adsorption materials. However, ZIF-8 as an adsorbent has a problem that separation by an adsorbent is difficult because ZIF-8 is small and has poor settling properties, and is generally separated in a laboratory by a high-speed centrifuge. The ZIF-8 is applied to actual wastewater treatment, and firstly the separation problem of an adsorbent needs to be solved, and the ZIF-8 and Filter Paper (FP) are compounded to form a composite adsorption material in the invention so as to solve the technical problem in the using process.
Disclosure of Invention
The invention solves the technical problem of providing a preparation method of a ZIF-8@ FP composite adsorption material and application thereof in adsorption and purification treatment of copper-containing wastewater, wherein the ZIF-8@ FP composite adsorption material successfully solves the problem of difficult separation when ZIF-8 is used alone as an adsorbent, and has good adsorption performance, strong adsorption selectivity, strong anti-interference capability, high adsorption rate and easy separation, and is suitable for adsorption and purification treatment of copper-containing wastewater.
The invention adopts the following technical scheme for solving the technical problems, and the preparation method of the ZIF-8@ FP composite adsorption material is characterized by comprising the following specific steps of: cutting filter paper into filter paper strips of 1cm by 4cm, placing the filter paper strips into a sodium hydroxide solution with the mass concentration of 10%, oscillating for 2 hours at the temperature of 30 ℃ and at the speed of 120r/min, washing the filter paper strips to be neutral by using distilled water, and drying the filter paper strips at the temperature of 60 ℃ to obtain pretreated filter paper for later use; 1.17g of Zn (NO)3)2·6H2Dissolving O in 8mL of distilled water, adding pretreated filter paper, soaking for 20min, dissolving 22.6g of 2-methylimidazole in 80mL of distilled water, pouring the formed 2-methylimidazole solution into the solution for soaking the filter paper, oscillating for 24h at 30 ℃ and 120r/min, standing for 24h, cleaning by using distilled water, and drying at 60 ℃ to obtain the ZIF-8@ FP composite adsorbing material.
The ZIF-8 of the inventionThe application of the @ FP composite adsorption material in the adsorption and purification treatment of copper-containing wastewater is characterized in that the specific process is as follows: putting a ZIF-8@ FP composite adsorption material in a Zn-metal ion2+、Cd2+、Ni2+、Mn2+、Co2+、 Mg2+And Cr6+And adsorbing the coexisting copper-containing wastewater for 180min at 30 ℃ to realize the adsorption and purification treatment of the copper-containing wastewater.
The preparation method of the ZIF-8@ FP composite adsorption material is simple in process, convenient to operate and mild in conditions, and the prepared ZIF-8@ FP composite adsorption material is high in adsorption selectivity, high in anti-interference capacity, high in adsorption rate, easy to separate and suitable for adsorption purification treatment of copper-containing wastewater.
Drawings
FIG. 1 is an infrared spectrum of ZIF-8;
FIG. 2 is an IR spectrum of FP;
FIG. 3 is an IR spectrum of ZIF-8@ FP;
FIG. 4 is an XRD spectrum of ZIF-8;
FIG. 5 is an XRD spectrum of FP;
FIG. 6 is an XRD spectrum of ZIF-8@ FP;
FIG. 7 is an SEM image of ZIF-8;
FIG. 8 is an SEM image of a FP;
FIG. 9 is an SEM image of ZIF-8@ FP;
FIG. 10 is a graph of the effect of equilibration time on adsorbed copper of ZIF-8@ FP;
FIG. 11 is a bar graph of adsorption selectivity of ZIF-8@ FP.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Examples
1. Preparation of ZIF-8@ FP composite adsorbing material:
preparation of pretreated Filter paper
Cutting the filter paper into filter paper strips of 1cm x 4cm, placing the filter paper strips into a sodium hydroxide solution with the mass concentration of 10%, oscillating for 2 hours at the temperature of 30 ℃ and at the speed of 120r/min, washing the filter paper strips to be neutral by using distilled water, and drying the filter paper strips at the temperature of 60 ℃ to obtain the pretreated filter paper for later use.
Preparation of ZIF-8@ FP
1.17g of Zn (NO)3)2·6H2Dissolving O in 8mL of distilled water, adding pretreated filter paper, soaking for 20min, dissolving 22.6g of 2-methylimidazole in 80mL of distilled water, pouring the formed 2-methylimidazole solution into the solution for soaking the filter paper, oscillating for 24h at 30 ℃ and 120r/min, standing for 24h, cleaning by using distilled water, and drying at 60 ℃ to obtain the ZIF-8@ FP composite adsorbing material. To demonstrate the successful synthesis and binding of ZIF-8 to filter paper, ZIF-8 was synthesized without filter paper and other conditions.
2. And (3) characterization:
FIGS. 1-3 are IR spectra of ZIF-8, FP and ZIF-8@ FP. ZIF-8 infrared spectrum at 1580cm-1The expansion vibration peak of C = N bond of imidazole ring appears at 421cm-1And a Zn-N bond stretching vibration peak appears, which indicates that the preparation of the ZIF-8 is successful. The ZIF-8@ FP infrared spectrum has a characteristic absorption peak of the filter paper infrared spectrum and is at 421cm-1A Zn-N bond stretching vibration peak is observed, which proves that ZIF-8@ FP is successfully prepared.
FIGS. 4-6 are XRD spectra of ZIF-8, FP and ZIF-8@ FP. An XRD spectrogram of the ZIF-8@ FP has a characteristic diffraction peak corresponding to the ZIF-8 and a characteristic diffraction peak corresponding to the filter paper, which shows that the synthesis of the ZIF-8@ FP does not damage the crystal structure of the ZIF-8.
FIGS. 7-9 are scanning electron micrographs of ZIF-8, FP and ZIF-8@ FP. The ZIF-8 particles are distributed uniformly, and the shape difference between the filter paper and the ZIF-8@ FP is large, which shows that the ZIF-8@ FP is prepared successfully.
3. Adsorption performance:
FIG. 10 is a graph of the effect of equilibration time on copper adsorption by ZIF-8@ FP. The experimental conditions are as follows: one ZIF-8@ FP composite adsorption material, Cu2+50mL of solution with the concentration of 50 mug/mL, the oscillation speed of 160r/min and the temperature of 30 ℃. The adsorption speed of the ZIF-8@ FP composite adsorption material on copper ions is high, and the adsorption capacity reaches 90% of the equilibrium adsorption capacity in 180minThe above.
FIG. 11 is a bar graph of adsorption selectivity of ZIF-8@ FP composite adsorbent material. The experimental conditions are as follows: the adsorbent is a ZIF-8@ FP composite adsorption material, the concentration of various metal ions is 50 mug/mL, the volume is 50mL, the balance time is 8h, the oscillation speed is 160r/min, and the temperature is 30 ℃. In Cu2+、Au3+、Pb2+、Zn2+、Cd2+、Ni2+、Mn2+、Co2+、Mg2+And Cr6+In the plasma metal ions, the ZIF-8@ FP composite adsorption material shows stronger adsorption selectivity and is used for Cu2+The adsorption amount of (A) is far greater than that of other metals.
Table 1 shows the adsorption of the ZIF-8@ FP composite adsorption material to copper when common metal ions and copper ions coexist. The adsorbent is a ZIF-8@ FP composite adsorption material, various metal ions and copper ions form a binary system respectively, the concentration of the metal ions and the copper ions is 50 mug/mL, the volume of the metal ions is 50mL, the balance time is 8h, the oscillation speed is 160r/min, and the temperature is 30 ℃. In Zn2+、Cd2+、Ni2+、Mn2+、Co2+、Mg2+And Cr6+Under the condition that metal ions and copper ions coexist respectively, the adsorption capacity of the ZIF-8@ FP composite adsorption material to the copper ions is not obviously reduced, and the adsorption capacity to common metals is very low, which shows that the anti-interference performance of the ZIF-8@ FP composite adsorption material to the copper ions is strong.
TABLE 1 anti-interference performance of ZIF-8@ FP copper adsorption

Claims (2)

1. A preparation method of a ZIF-8@ FP composite adsorption material is characterized by comprising the following specific steps: cutting filter paper into filter paper strips of 1cm by 4cm, placing the filter paper strips into a sodium hydroxide solution with the mass concentration of 10%, oscillating for 2 hours at the temperature of 30 ℃ and at the speed of 120r/min, washing the filter paper strips to be neutral by using distilled water, and drying the filter paper strips at the temperature of 60 ℃ to obtain pretreated filter paper for later use; 1.17g of Zn (NO)3)2·6H2Dissolving O in 8mL of distilled water, and adding the pretreated filter paperSoaking for 20min, dissolving 22.6g of 2-methylimidazole in 80mL of distilled water, pouring the formed 2-methylimidazole solution into a solution for soaking filter paper, oscillating for 24h at 30 ℃ and 120r/min, standing for 24h, cleaning by using distilled water, and drying at 60 ℃ to obtain the ZIF-8@ FP composite adsorbing material which is prepared by soaking the ZIF-8@ FP composite adsorbing material in Cu2+、Au3+、Pb2+、Zn2+、Cd2+、Ni2+、Mn2+、Co2+、Mg2+And Cr6+In metal ions, the ZIF-8@ FP composite adsorption material shows strong adsorption selectivity and has Cu resistance2+The adsorption amount of (A) is far greater than that of other metals.
2. The application of the ZIF-8@ FP composite adsorption material prepared by the method according to claim 1 in the adsorption and purification treatment of copper-containing wastewater is characterized by comprising the following specific steps: putting a ZIF-8@ FP composite adsorption material in a Zn-metal ion2+、Cd2+、Ni2 +、Mn2+、Co2+、 Mg2+And Cr6+And adsorbing the coexisting copper-containing wastewater for 180min at 30 ℃ to realize the adsorption and purification treatment of the copper-containing wastewater.
CN201710764914.9A 2017-08-30 2017-08-30 Preparation method of ZIF-8@ FP composite adsorption material and application of adsorption material in adsorption and purification treatment of copper-containing wastewater Expired - Fee Related CN107486164B (en)

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CN108589399B (en) * 2018-05-11 2019-10-29 陕西科技大学 One kind being based on cellulose base/ZIF-8 composite material and preparation method
CN109046257A (en) * 2018-08-31 2018-12-21 河南师范大学 It is a kind of for adsorbing the FeCl of fluorine ion3The preparation method and applications of modified ZIF-8 compound adsorbent
CN109174018B (en) * 2018-10-26 2022-12-02 吉林大学 Hg (II) monolithic adsorption material and method for removing Hg (II) in water
CN109731555B (en) * 2019-03-04 2022-03-25 长春工业大学 For CO2Preparation method and application of adsorbed ZIF-8/shaddock peel composite material

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