CN105879841A - SiO2@PDA@ZIF-8 composite adsorbent for selectively adsorbing lead ions in wastewater and preparing method thereof - Google Patents

SiO2@PDA@ZIF-8 composite adsorbent for selectively adsorbing lead ions in wastewater and preparing method thereof Download PDF

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Publication number
CN105879841A
CN105879841A CN201610371682.6A CN201610371682A CN105879841A CN 105879841 A CN105879841 A CN 105879841A CN 201610371682 A CN201610371682 A CN 201610371682A CN 105879841 A CN105879841 A CN 105879841A
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pda
zif
sio
compound adsorbent
dopamine
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CN105879841B (en
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王治科
陈凌云
陈海天
叶存玲
范顺利
李倩霞
段亚云
刘菲
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Henan Normal University
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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
    • B01J20/02—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
    • 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
    • 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]
    • 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
    • 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 & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • 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

The invention discloses a SiO2@PDA@ZIF-8 composite adsorbent for selectively adsorbing lead ions in wastewater and a preparing method thereof, and belongs to the technical field of synthesis of silica gel composite adsorbents. According to the technical scheme, the preparing method includes the steps that activated silica gel is added into a Tris-HCL buffered solution with dissolved dopamine hydrochloride to obtain dopamine-modified silica gel SiO2@PDA; a methanol solution of zinc nitrate hexahydrate is added into a methanol solution of 2-methylimidazole and sodium formate, then the dopamine-modified silica gel SiO2@PDA is added, the mixture is stirred and reacted at the temperature of 85 DEG C, and the SiO2@PDA@ZIF-8 composite adsorbent is obtained. According to the SiO2@PDA@ZIF-8 composite adsorbent and the preparing method, the number of synergistic steps of the preparing process is small, the technology is reliable, and the prepared SiO2@PDA@ZIF-8 composite adsorbent is large in lead ion absorption quantity and high anti-interference capacity, and can be used for selectively adsorbing lead ions in wastewater.

Description

A kind of SiO for selective absorption Pb In Exhausted Water ion2@PDA@ZIF-8 is compound to be inhaled Attached dose and preparation method thereof
Technical field
The invention belongs to the synthesis technical field of silica gel composite absorbent, be specifically related to a kind of for selective absorption waste water The SiO of middle lead ion2@PDA@ZIF-8 compound adsorbent and preparation method thereof.
Background technology
Lead belongs to priority pollutants in water, lead waste water wide material sources, thus the health of human body is constituted potential prestige The side of body.At present, the method for lead in water of removing has ion-exchange, chemical precipitation method and absorption method etc..Wherein, absorption method has because of it The advantage such as easy and simple to handle and efficient, the most extensively applies.But, it is critical only that of absorption method is developed lead suction Attached amount the strongest material high, selective is as adsorbent.
Summary of the invention
Present invention solves the technical problem that and there is provided that a kind of lead ion adsorbance is high and selectivity is stronger for selecting The SiO of property Adsorbing Lead Ion in Polluted Water2@PDA@ZIF-8 compound adsorbent and preparation method thereof.
The present invention solves that above-mentioned technical problem adopts the following technical scheme that, a kind of for selective absorption Pb In Exhausted Water The SiO of ion2The preparation method of@PDA@ZIF-8 compound adsorbent, it is characterised in that: first activated silica gel is joined dissolving Have in the Tris-HCl cushioning liquid of dopamine hydrochloride and obtain dopamine modified silica-gel SiO2@PDA；Then by zinc nitrate hexahydrate Methanol solution join in the methanol solution of 2-methylimidazole and sodium formate, add dopamine modified silica-gel SiO2@PDA, SiO is prepared in 85 DEG C of stirring reactions2@PDA@ZIF-8 compound adsorbent.
SiO for selective absorption Pb In Exhausted Water ion of the present invention2The system of@PDA@ZIF-8 compound adsorbent Preparation Method, it is characterised in that concretely comprise the following steps:
Step (1), dopamine modified silica-gel SiO2The synthesis of@PDA, 400mg dopamine hydrochloride is dissolved in 200mL pH value is In the Tris-HCl cushioning liquid of 8.5, adding 200mg activated silica gel, magnetic agitation 20h under room temperature, centrifugation also uses second Alcohol obtains dopamine modified silica-gel SiO in 50 DEG C of vacuum drying 12h after repeatedly washing2@PDA；
Step (2), SiO2The synthesis of@PDA@ZIF-8 compound adsorbent, is dissolved in 100mL methyl alcohol by 3.522g zinc nitrate hexahydrate molten In liquid, then 1.944g 2-methylimidazole and 0.804g sodium methoxide are dissolved in 50mL methanol solution, then by zinc nitrate hexahydrate Methanol solution joins in the methanol solution of 2-methylimidazole and sodium formate, adds the dopamine that 200mg step (1) obtains and changes Property silica gel SiO2@PDA, reacts 24h, stratification after reaction completely in 85 DEG C of magnetic agitation, topples over upper solution, again with methanol Wash three times, obtain SiO in 25 DEG C of vacuum drying 12h2@PDA@ZIF-8 compound adsorbent.
SiO for selective absorption Pb In Exhausted Water ion of the present invention2@PDA@ZIF-8 compound adsorbent, it is special Levy and be to prepare according to the method described above.
SiO for selective absorption Pb In Exhausted Water ion of the present invention2Answering of@PDA@ZIF-8 compound adsorbent With, it is characterised in that detailed process is: add 20mg in the waste water that 50mL lead ion mass concentration is 50-120 μ g/mL SiO2@PDA@ZIF-8 compound adsorbent, reaches adsorption equilibrium in 30 DEG C, and the adsorption rate of Pb In Exhausted Water ion reaches more than 91%.
The present invention compared with prior art has the advantages that SiO2The preparation of@PDA@ZIF-8 compound adsorbent Journey synthesis step is less, process, prepared SiO2@PDA@ZIF-8 compound adsorbent is big to the adsorbance of lead ion, anti-dry Disturb ability strong, it is possible to the lead ion in selective absorption waste water.
Accompanying drawing explanation
Fig. 1 is the dopamine modified silica-gel SiO that the embodiment of the present invention 1 prepares2The infrared spectrogram of@PDA；
Fig. 2 is the SiO that the embodiment of the present invention 1 prepares2The infrared spectrogram of@PDA@ZIF-8 compound adsorbent；
Fig. 3 is the SiO that the embodiment of the present invention 1 prepares2The XRD spectrum of@PDA@ZIF-8 compound adsorbent and ZIF-8；
Fig. 4 is the dopamine modified silica-gel SiO that the embodiment of the present invention 1 prepares2The SEM figure of@PDA；
Fig. 5 is the SiO that the embodiment of the present invention 1 prepares2The SEM figure of@PDA@ZIF-8 compound adsorbent；
Fig. 6 be in the embodiment of the present invention 3 plumbum ion concentration to SiO2The adsorption rate influence curve of@PDA@ZIF-8 compound adsorbent；
Fig. 7 be in the embodiment of the present invention 4 time to SiO2The adsorption rate influence curve of@PDA@ZIF-8 compound adsorbent.
Detailed description of the invention
By the following examples the foregoing of the present invention is described in further details, but this should be interpreted as this The scope inventing above-mentioned theme is only limitted to below example, and all technology realized based on foregoing of the present invention belong to this Bright scope.
Embodiment 1
SiO for selective absorption Pb In Exhausted Water ion2The synthesis of@PDA@ZIF-8 compound adsorbent
1,400mg dopamine hydrochloride is dissolved in the Tris-HCl cushioning liquid that 200mL pH value is 8.5, adds 200mg Activated silica gel, magnetic agitation 20h under room temperature, centrifugation also obtains many in 50 DEG C of vacuum drying 12h after repeatedly washing with ethanol Bar amine modified silica-gel SiO2@PDA；
2,3.522g zinc nitrate hexahydrate is dissolved in 100mL methanol solution, then by 1.944g 2-methylimidazole and 0.804g methyl alcohol Sodium is dissolved in 50mL methanol solution, and then the methanol solution of zinc nitrate hexahydrate joins the methyl alcohol of 2-methylimidazole and sodium formate In solution, add 200mg dopamine modified silica-gel SiO2@PDA, reacts 24h in 85 DEG C of magnetic agitation, stands after reaction completely Layering, topples over upper solution, and again with methanol is washed three times, obtains SiO in 25 DEG C of vacuum drying 12h2@PDA@ZIF-8 is compound to be inhaled Attached dose.
Fig. 1 is the dopamine modified silica-gel SiO of the present embodiment synthesis2The infrared spectrogram of@PDA, 1508cm in figure-1With 1605cm-1The absworption peak at place proves the success of dopamine modified silica-gel.
Fig. 2 is the SiO of the present embodiment synthesis2The infrared spectrogram of@PDA@ZIF-8 compound adsorbent, 3135cm in figure-1With 2930cm-1The absworption peak at place proves ZIF-8 success modified silica-gel.
Fig. 3 is respectively the SiO of the present embodiment synthesis2The XRD spectrum of@PDA@ZIF-8 compound adsorbent and ZIF-8, in figure SiO2@PDA@ZIF-8 compound adsorbent is consistent with the XRD spectra of ZIF-8, and this shows that both have consistent crystal structure, logical Crossing poly-dopamine and realize ZIF-8 modified silica-gel, the crystal structure of ZIF-8 does not destroy.
Fig. 4 is the dopamine modified silica-gel SiO of the present embodiment synthesis2The SEM figure of@PDA, Fig. 5 is the present embodiment synthesis SiO2The SEM figure of@PDA@ZIF-8 compound adsorbent, its pattern is significantly different as seen from the figure, and then proves that ZIF-8 successfully modifies Silica gel.
Embodiment 2
Interference experiment
Pb2+It is 100 μ g/mL with coexistent metallic ion concentration, simulates Pb respectively2+-Cu2+, Pb2+-Cd2+, Pb2+-Mn2+, Pb2+- Mg2+, Pb2+-Co2+, Pb2+-Zn2+Coexist system on lead and other metal, at solution 50mL, 20mg SiO2@PDA@ZIF-8 is combined Adsorbent, 30 DEG C, vibration absorption 7h under conditions of 160r/min, result is as shown in table 1, common metal ion such as Cu2+、Cd2+、 Mn2+、Mg2+、Co2+、Zn2+Deng to SiO2@PDA@ZIF-8 Composite Adsorbent Absorbing Pb2+Almost without interference, and except to Cu2+ Adsorbance be outside 153mg/g, SiO2@PDA@ZIF-8 compound adsorbent adsorbs Cd hardly2+、Mn2+、Mg2+、Co2+、Zn2+Deng Other coexistent metallic ion.
Table 1 interference test result
Embodiment 3
Initial concentration is to SiO2The impact of@PDA@ZIF-8 Composite Adsorbent Absorbing rate
50mL contains Pb2+Solution, 20mg SiO2@PDA@ZIF-8 compound adsorbent, 30 DEG C, under conditions of 160r/min vibration inhale Attached, different Pb2+The initial concentration impact on its clearance.As shown in Figure 6, in 50-120 μ g/mL concentration range, lead ion Eliminating rate of absorption, all more than 91%, shows SiO2@PDA@ZIF-8 compound adsorbent is suitable for Adsorption low concentration lead waste water.
Embodiment 4
Time is to SiO2The impact of@PDA@ZIF-8 Composite Adsorbent Absorbing rate
50mL contains Pb2+Solution, 20mg SiO2@PDA@ZIF-8 compound adsorbent, 30 DEG C, under conditions of 160r/min vibration inhale Attached.As shown in Figure 7, under conditions of low concentration 50 μ g/mL, 60min absorption reaches balance.
Embodiment above describes the general principle of the present invention, principal character and advantage, the technical staff of the industry should Understanding, the present invention is not restricted to the described embodiments, and the simply explanation present invention's described in above-described embodiment and specification is former Reason, under the scope without departing from the principle of the invention, the present invention also has various changes and modifications, and these changes and improvements each fall within In the scope of protection of the invention.

Claims (4)

1. the SiO for selective absorption Pb In Exhausted Water ion2The preparation method of@PDA@ZIF-8 compound adsorbent, it is special Levy and be: first join activated silica gel to be dissolved with and the Tris-HCl cushioning liquid of dopamine hydrochloride obtains dopamine change Property silica gel SiO2@PDA；Then the methanol solution of zinc nitrate hexahydrate is joined the methanol solution of 2-methylimidazole and sodium formate In, add dopamine modified silica-gel SiO2@PDA, prepares SiO in 85 DEG C of stirring reactions2@PDA@ZIF-8 compound adsorbent.
SiO for selective absorption Pb In Exhausted Water ion the most according to claim 12@PDA@ZIF-8 compound adsorbent Preparation method, it is characterised in that concretely comprise the following steps:
Step (1), dopamine modified silica-gel SiO2The synthesis of@PDA, 400mg dopamine hydrochloride is dissolved in 200mL pH value is In the Tris-HCl cushioning liquid of 8.5, adding 200mg activated silica gel, magnetic agitation 20h under room temperature, centrifugation also uses second Alcohol obtains dopamine modified silica-gel SiO in 50 DEG C of vacuum drying 12h after repeatedly washing2@PDA；
Step (2), SiO2The synthesis of@PDA@ZIF-8 compound adsorbent, is dissolved in 100mL methanol solution by 3.522g zinc nitrate hexahydrate In, then 1.944g 2-methylimidazole and 0.804g sodium methoxide are dissolved in 50mL methanol solution, then by the first of zinc nitrate hexahydrate Alcoholic solution joins in the methanol solution of 2-methylimidazole and sodium formate, adds the dopamine modification that 200mg step (1) obtains Silica gel SiO2@PDA, reacts 24h, stratification after reaction completely in 85 DEG C of magnetic agitation, topples over upper solution, and again with methanol is washed Wash three times, obtain SiO in 25 DEG C of vacuum drying 12h2@PDA@ZIF-8 compound adsorbent.
3. the SiO for selective absorption Pb In Exhausted Water ion2@PDA@ZIF-8 compound adsorbent, it is characterised in that according to Method described in claim 1 or 2 prepares.
4. the SiO for selective absorption Pb In Exhausted Water ion described in claim 32Answering of@PDA@ZIF-8 compound adsorbent With, it is characterised in that detailed process is: add 20mg in the waste water that 50mL lead ion mass concentration is 50-120 μ g/mL SiO2@PDA@ZIF-8 compound adsorbent, reaches adsorption equilibrium in 30 DEG C, and the adsorption rate of Pb In Exhausted Water ion reaches more than 91%.
CN201610371682.6A 2016-05-31 2016-05-31 A kind of SiO2@PDA@ZIF-8 compound adsorbent and preparation method thereof for selective absorption Pb In Exhausted Water ion Expired - Fee Related CN105879841B (en)

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CN107088403A (en) * 2017-06-07 2017-08-25 河南师范大学 A kind of thiosemicarbazides bonding PDA@MWCNTs adsorbents and its preparation method and application
CN107519848A (en) * 2017-10-18 2017-12-29 福州大学 Poly-dopamine cladding silica gel that a kind of polyethylene polyamine is modified and its preparation method and application
CN108993446A (en) * 2018-09-06 2018-12-14 苏州佰锐生物科技有限公司 A kind of preparation method of adsorbent for heavy metal
CN109012595A (en) * 2018-09-06 2018-12-18 苏州佰锐生物科技有限公司 A kind of preparation method of modified carbon nano-tube adsorbent for heavy metal
CN109052541A (en) * 2018-09-06 2018-12-21 苏州佰锐生物科技有限公司 A method of removal heavy metal in waste water nickel ion
CN109052542A (en) * 2018-09-06 2018-12-21 苏州佰锐生物科技有限公司 A kind of preparation method for the modified carbon nano-tube removing mercury ions in waste water
CN110604132A (en) * 2019-09-26 2019-12-24 吉林大学 Preparation method of hollow core-satellite-shaped poly-dopamine silver-loaded antibacterial nanocapsule
CN111073139A (en) * 2019-12-23 2020-04-28 重庆普利特新材料有限公司 Anti-aging, low-odor and low-emission modified polypropylene composite material for vehicles and preparation method thereof
CN111792649A (en) * 2020-07-15 2020-10-20 浙江爱津生物技术有限公司 Preparation method of modified silica gel membrane for nucleic acid detection
CN111905816A (en) * 2020-07-08 2020-11-10 武汉纺织大学 ZIF-8 functional fabric and preparation method thereof
CN112516968A (en) * 2020-12-16 2021-03-19 东北电力大学 Preparation method of metal organic framework material loaded modified diatomite adsorbent
CN112979979A (en) * 2021-02-23 2021-06-18 云南省水利水电科学研究院 Preparation method and application of modified ZIF-8 material for adsorbing and removing micro-polluted mercury in water body
CN113244898A (en) * 2021-05-27 2021-08-13 江西理工大学 Polydopamine-kaolin-Fe3O4Composite material and preparation method and application thereof
CN113877549A (en) * 2021-08-17 2022-01-04 福州大学 Selective composite microsphere adsorption material and preparation method and application thereof
WO2023236317A1 (en) * 2022-06-10 2023-12-14 大连科利德光电子材料有限公司 Impurity adsorbent, preparation method and method for using adsorbent to purify trimethylaluminium

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CN107088403B (en) * 2017-06-07 2019-11-05 河南师范大学 A kind of thiosemicarbazides bonding PDA@MWCNTs adsorbent and its preparation method and application
CN107088403A (en) * 2017-06-07 2017-08-25 河南师范大学 A kind of thiosemicarbazides bonding PDA@MWCNTs adsorbents and its preparation method and application
CN107519848A (en) * 2017-10-18 2017-12-29 福州大学 Poly-dopamine cladding silica gel that a kind of polyethylene polyamine is modified and its preparation method and application
CN108993446A (en) * 2018-09-06 2018-12-14 苏州佰锐生物科技有限公司 A kind of preparation method of adsorbent for heavy metal
CN109012595A (en) * 2018-09-06 2018-12-18 苏州佰锐生物科技有限公司 A kind of preparation method of modified carbon nano-tube adsorbent for heavy metal
CN109052541A (en) * 2018-09-06 2018-12-21 苏州佰锐生物科技有限公司 A method of removal heavy metal in waste water nickel ion
CN109052542A (en) * 2018-09-06 2018-12-21 苏州佰锐生物科技有限公司 A kind of preparation method for the modified carbon nano-tube removing mercury ions in waste water
CN110604132B (en) * 2019-09-26 2021-10-08 吉林大学 Preparation method of hollow core-satellite-shaped poly-dopamine silver-loaded antibacterial nanocapsule
CN110604132A (en) * 2019-09-26 2019-12-24 吉林大学 Preparation method of hollow core-satellite-shaped poly-dopamine silver-loaded antibacterial nanocapsule
CN111073139A (en) * 2019-12-23 2020-04-28 重庆普利特新材料有限公司 Anti-aging, low-odor and low-emission modified polypropylene composite material for vehicles and preparation method thereof
CN111073139B (en) * 2019-12-23 2022-04-08 重庆普利特新材料有限公司 Anti-aging, low-odor and low-emission modified polypropylene composite material for vehicles and preparation method thereof
CN111905816A (en) * 2020-07-08 2020-11-10 武汉纺织大学 ZIF-8 functional fabric and preparation method thereof
CN111792649A (en) * 2020-07-15 2020-10-20 浙江爱津生物技术有限公司 Preparation method of modified silica gel membrane for nucleic acid detection
CN112516968A (en) * 2020-12-16 2021-03-19 东北电力大学 Preparation method of metal organic framework material loaded modified diatomite adsorbent
CN112979979A (en) * 2021-02-23 2021-06-18 云南省水利水电科学研究院 Preparation method and application of modified ZIF-8 material for adsorbing and removing micro-polluted mercury in water body
CN113244898A (en) * 2021-05-27 2021-08-13 江西理工大学 Polydopamine-kaolin-Fe3O4Composite material and preparation method and application thereof
CN113877549A (en) * 2021-08-17 2022-01-04 福州大学 Selective composite microsphere adsorption material and preparation method and application thereof
WO2023236317A1 (en) * 2022-06-10 2023-12-14 大连科利德光电子材料有限公司 Impurity adsorbent, preparation method and method for using adsorbent to purify trimethylaluminium

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