CN109647355A - A kind of preparation method of the efficient adsorbents for lead ion pyrolytic of growth in situ manganese dioxide - Google Patents
A kind of preparation method of the efficient adsorbents for lead ion pyrolytic of growth in situ manganese dioxide Download PDFInfo
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- CN109647355A CN109647355A CN201811529517.4A CN201811529517A CN109647355A CN 109647355 A CN109647355 A CN 109647355A CN 201811529517 A CN201811529517 A CN 201811529517A CN 109647355 A CN109647355 A CN 109647355A
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- B01J20/26—Synthetic macromolecular compounds
Abstract
The present invention relates to a kind of preparation methods of efficient adsorbents for lead ion pyrolytic of growth in situ manganese dioxide, it is after preparing redox graphene doping ultra-fine polymer nano fibrous membrane by electrostatic spinning, it is grown obtained by one layer of manganese dioxide in its surface in situ, its feature includes the configuration of 1) spinning solution, 2) electrostatic spinning, 3) Situ Hydrothermal growth three steps of manganese dioxide.Nano-fibre supported type adsorbent produced by the present invention has compared with high adsorption lead ion, has broad application prospects in heavy metal ion field.
Description
Technical field
The present invention relates to a kind of preparation methods of efficient adsorbents for lead ion pyrolytic of growth in situ manganese dioxide, and in particular in conjunction with
Electrostatic spinning technique and hydrothermal growth prepare a kind of fine polymer nano fibrous membrane load manganese dioxide (MnO2) efficient lead
The preparation method of ion adsorbent belongs to functional high molecular fibre technical field.
Technical background
Nano-metal-oxide has a wide range of applications in removal of heavy metal ions field, mainly includes Fe2O3、Fe3O4、
ZnO、Al2O3、CeO2、MnO2、Mn3O4Equal nano-oxides.Wherein, nanometer MnO2Due to biggish specific surface area, surface
There is stronger adsorptivity to heavy metal ion with microcellular structure and containing great amount of hydroxy group, and then obtained the wide of researcher
General concern.However, in practical adsorption process, nanometer MnO2Due to surface energy with higher, easily reunite；Meanwhile how
By the nanometer MnO after absorption2It is still a problem to be solved that adsorbent is separated from water body.
In order to solve this problem,Etc. first reported a kind of cellulose acetate load MnO2Adsorbent, this
It can be easy to separate (BRAND O M S B.GALEMBECK F.Copper, lead from solution after kind adsorbent absorption
and zinc adsorption on MnO2-impregnated cellulose acetate[J].Colloids&
Surfaces, 1990,48 (4): 351-362.).Luo et al. develops a kind of by MnO2Nanoparticle spontaneously deposits to poly- third
Then the method on alkene nitrile nanofibre surface passes through poly- pyrrole that is, first in one strata pyrroles of polyacrylonitrile nanofiber surface aggregate
The redox reaction between potassium permanganate is coughed up by the MnO of generation2Nanoparticle deposit to nanofiber surface (LUO C,
WANG J Q, JIA P, et al.Hierarchically structured polyacrylonitrile nanofiber
mat as highly efficient lead adsorbent for water treatment[J].Chemical
Engineering Journal, 2015,262:775-784.).
The present invention inquires into out a kind of fine polymer nano fibrous membrane growth in situ MnO2The preparation method of adsorbent.Pass through
The adsorbent of this method preparation is because it is with biggish specific surface area and MnO2The homoepitaxial of nanometer sheet makes it have excellent
Lead ion absorption property.Here is specific summary of the invention.
Summary of the invention
The present invention relates to a kind of fine polymer nano fibrous membrane growth in situ MnO2The preparation method of adsorbent, using this
The technical solution of invention can prepare a kind of efficient adsorbents for lead ion pyrolytic, ultra-fine to be capable of providing biggish specific surface area, reduction
The introducing of graphene oxide (RGO) can make MnO2Nanometer sheet is uniformly grown in fiber surface, and then provides more for adsorbent
More active sites.Superfine nano tunica fibrosa growth in situ MnO prepared by the present invention2Adsorbent is in heavy metal ion adsorbed neck
Domain has broad application prospects.
A kind of preparation method of efficient adsorbents for lead ion pyrolytic of growth in situ manganese dioxide of the present invention, feature exist
In, comprising:
(1) configuration of spinning solution: a certain amount of redox graphene powder is added to containing a certain amount of four hexyls bromination
In the high polymeric solution of ammonium, ultrasonic disperse 0.5h obtains electrostatic spinning liquid；The high polymer is cellulose acetate, nylon 6；
The high polymeric solution concentration is 8~20%；The redox graphene accounts for the polymer dope quality percentage
Than being 0.1~0.3%；The four hexyl bromination ammonium concentrations are 0.05~0.15mol L-1；
(2) previous step spinning solution electrostatic spinning: is subjected to spinning, at room temperature, relative humidity 20 using method of electrostatic spinning
± 10%, spinning voltage is 15~35kV, and receiving distance is 10~20cm, and feed flow rate is 0.5~1.5mL/h, and reduction is made
Graphene oxide doped ultra-fine polymer nano fibrous membrane；
(3) growth in situ manganese dioxide: a certain amount of potassium permanganate is dissolved into deionized water, fibre prepared by previous step
It ties up film to take out, be added in liquor potassic permanganate；It is added dropwise into above-mentioned solution after 1h is stirred at room temperature in a certain amount of concentrated sulfuric acid, it will be above-mentioned
Mixture is transferred to hydrothermal reaction kettle, 60 DEG C of reaction 6h, and reaction terminates, and tunica fibrosa taking-up deionized water repeated flushing is dried
It is dry, growth in situ manganese dioxide adsorbents for lead ion pyrolytic is made；The mass fraction 0.01~0.1% of the liquor potassic permanganate；
The mass percent that the concentrated sulfuric acid accounts for the liquor potassic permanganate is 1~3%.
It states technical solution and can be seen that the present invention and ultra-fine polymer nano fibrous membrane is prepared using electrospinning process,
By the way that RGO is added in spinning solution, redox reaction, the MnO of generation then occur between RGO and potassium permanganate2Nanometer sheet
It is uniformly grown in its surface, so that superfine nano tunica fibrosa growth in situ MnO be made2Adsorbent.The adsorbent is to lead ion
Adsorptivity with higher and reusability.
Advantages of the present invention is as follows compared with prior art:
(1) present invention uses a step electrostatic spinning technique, by the way that a certain amount of four hexyls bromination is added into polymer solution
Ammonium prepares fine polymer nano fibrous membrane, and wherein minimum fiber diameter can reach 5nm, and it is with higher to assign the tunica fibrosa
Specific surface area.
(2) present invention is by being added a certain amount of RGO into spinning solution, and in hydrothermal reaction process, RGO and potassium permanganate occur
Redox reaction, to make MnO2Nanometer sheet is uniformly grown in fiber surface.
(3) superfine nano tunica fibrosa growth in situ MnO provided by the present invention2Adsorbent is to lead ion suction with higher
Attached property, and there is good recycling.
Picture and text are briefly described
Fig. 1 is the ultra-fine nylon 6/nanometer fiber growth in situ MnO prepared using the embodiment of the present invention 12Adsorbent is swept
Retouch Electronic Speculum schematic diagram.
Fig. 2 is the ultra-fine cellulose acetate nanofiber growth in situ MnO prepared using the embodiment of the present invention 52Absorption
The scanning electron microscope schematic diagram of agent.
Specific embodiment
Embodiment 1
(1) configuration of spinning solution: 50mg redox graphene powder is taken to be added to containing tetra- hexyl ammonium bromide of 1.0g
In 6 solution of nylon that mass fraction is 18%, ultrasonic disperse 0.5h obtains electrostatic spinning liquid；
(2) previous step spinning solution electrostatic spinning: is subjected to spinning, spinning technology parameter are as follows: room temperature using method of electrostatic spinning
Under, relative humidity is 20 ± 5%, spinning voltage 30kV, and receiving distance is 15cm, and feed flow rate is 1.0mL/h, and reduction is made
The ultra-fine nylon 6/nanometer tunica fibrosa of graphene oxide doped；
(3) growth in situ manganese dioxide: 0.13g potassium permanganate is dissolved into 30mL deionized water, is prepared by previous step
Tunica fibrosa take out, be added in liquor potassic permanganate；It, will be upper after into above-mentioned solution, 1h is stirred at room temperature in the dropwise addition 0.7g concentrated sulfuric acid
It states mixture and is transferred to hydrothermal reaction kettle, 60 DEG C of reaction 6h, reaction terminates, by tunica fibrosa taking-up deionized water repeated flushing,
Growth in situ MnO is made in drying2Adsorbents for lead ion pyrolytic.Fig. 1 is the ultra-fine nylon 6/nanometer prepared using the embodiment of the present invention 1
Fiber growth in situ MnO2The scanning electron microscope schematic diagram of adsorbent.10mg adsorbent obtained above is taken, 30mL concentration is added to
For the Pb of 100mg/L2+Adsorption liquid；Adsorption temp is 25 DEG C；Adsorption time is for 24 hours；Adsorption liquid pH value is 6.After the completion of absorption, adopt
With residue Pb in icp ms (ICP, Varian 715-ES, Varian company, the U.S.) test solution2+'s
Concentration obtains the adsorbent to Pb2+Adsorbance be 308.6mg/g.
Embodiment 2
(1) configuration of spinning solution: 100mg redox graphene powder is taken to be added to containing tetra- hexyl ammonium bromide of 1.5g
In 6 solution of nylon that mass fraction is 14%, ultrasonic disperse 0.5h obtains electrostatic spinning liquid；
(2) previous step spinning solution electrostatic spinning: is subjected to spinning, spinning technology parameter are as follows: room temperature using method of electrostatic spinning
Under, relative humidity is 20 ± 5%, spinning voltage 35kV, and receiving distance is 15cm, and feed flow rate is 0.6mL/h, and reduction is made
The ultra-fine nylon 6/nanometer tunica fibrosa of graphene oxide doped；
(3) growth in situ manganese dioxide: 0.25g potassium permanganate is dissolved into 30mL deionized water, is prepared by previous step
Tunica fibrosa take out, be added in liquor potassic permanganate；It, will be upper after into above-mentioned solution, 1h is stirred at room temperature in the dropwise addition 1.3g concentrated sulfuric acid
It states mixture and is transferred to hydrothermal reaction kettle, 60 DEG C of reaction 6h, reaction terminates, by tunica fibrosa taking-up deionized water repeated flushing,
Growth in situ MnO is made in drying2Adsorbents for lead ion pyrolytic.10mg adsorbent obtained above is taken, being added to 30mL concentration is
The Pb of 100mg/L2+Adsorption liquid；Adsorption temp is 25 DEG C；Adsorption time is for 24 hours；Adsorption liquid pH value is 6.After the completion of absorption, use
Icp ms (ICP, Varian 715-ES, Varian company, the U.S.) test residue Pb in solution2+It is dense
Degree, obtains the adsorbent to Pb2+Adsorbance be 328.7mg/g.
Embodiment 3
(1) configuration of spinning solution: 60mg redox graphene powder is taken to be added to containing tetra- hexyl ammonium bromide of 0.8g
In the cellulose acetate solution that mass fraction is 9%, ultrasonic disperse 0.5h obtains electrostatic spinning liquid；
(2) previous step spinning solution electrostatic spinning: is subjected to spinning, spinning technology parameter are as follows: room temperature using method of electrostatic spinning
Under, relative humidity is 40 ± 10%, spinning voltage 40kV, and receiving distance is 15cm, and feed flow rate is 0.8mL/h, is made also
The former ultra-fine cellulose acetate nano fibrous membrane of graphene oxide doped；
(3) growth in situ manganese dioxide: with embodiment 1.10mg adsorbent obtained above is taken, being added to 30mL concentration is
The Pb of 100mg/L2+Adsorption liquid；Adsorption temp is 25 DEG C；Adsorption time is for 24 hours；Adsorption liquid pH value is 6.After the completion of absorption, use
Icp ms (ICP, Varian 715-ES, Varian company, the U.S.) test residue Pb in solution2+It is dense
Degree, obtains the adsorbent to Pb2+Adsorbance be 343.6mg/g.
Embodiment 4
(1) configuration of spinning solution: 80mg redox graphene powder is taken to be added to containing tetra- hexyl ammonium bromide of 0.8g
In 6 solution of nylon that mass fraction is 16%, ultrasonic disperse 0.5h obtains electrostatic spinning liquid；
(2) previous step spinning solution electrostatic spinning: is subjected to spinning, spinning technology parameter are as follows: room temperature using method of electrostatic spinning
Under, relative humidity is 20 ± 5%, spinning voltage 30kV, and receiving distance is 15cm, and feed flow rate is 0.5mL/h, and reduction is made
The ultra-fine nylon 6/nanometer tunica fibrosa of graphene oxide doped；
(3) growth in situ manganese dioxide: 0.05g potassium permanganate is dissolved into 30mL deionized water, is prepared by previous step
Tunica fibrosa take out, be added in liquor potassic permanganate；It, will after into above-mentioned solution, 1h is stirred at room temperature in the dropwise addition 0.27g concentrated sulfuric acid
Said mixture is transferred to hydrothermal reaction kettle, 60 DEG C of reaction 6h, and reaction terminates, tunica fibrosa taking-up is rushed repeatedly with deionized water
It washes, dries, growth in situ MnO is made2Adsorbents for lead ion pyrolytic.10mg adsorbent obtained above is taken, being added to 30mL concentration is
The Pb of 100mg/L2+Adsorption liquid；Adsorption temp is 25 DEG C；Adsorption time is for 24 hours；Adsorption liquid pH value is 6.After the completion of absorption, use
Icp ms (ICP, Varian 715-ES, Varian company, the U.S.) test residue Pb in solution2+It is dense
Degree, obtains the adsorbent to Pb2+Adsorbance be 258.7mg/g.
Embodiment 5
(1) configuration of spinning solution: 150mg redox graphene powder is taken to be added to containing tetra- hexyl ammonium bromide of 0.5g
In the cellulose acetate solution that mass fraction is 11%, ultrasonic disperse 0.5h obtains electrostatic spinning liquid；
(2) previous step spinning solution electrostatic spinning: is subjected to spinning, spinning technology parameter are as follows: room temperature using method of electrostatic spinning
Under, relative humidity is 20 ± 5%, spinning voltage 40kV, and receiving distance is 15cm, and feed flow rate is 0.6mL/h, and reduction is made
The ultra-fine cellulose acetate nano fibrous membrane of graphene oxide doped；
(3) growth in situ manganese dioxide: 0.10g potassium permanganate is dissolved into 30mL deionized water, is prepared by previous step
Tunica fibrosa take out, be added in liquor potassic permanganate；It, will be upper after into above-mentioned solution, 1h is stirred at room temperature in the dropwise addition 0.3g concentrated sulfuric acid
It states mixture and is transferred to hydrothermal reaction kettle, 60 DEG C of reaction 6h, reaction terminates, by tunica fibrosa taking-up deionized water repeated flushing,
Growth in situ MnO is made in drying2Adsorbents for lead ion pyrolytic.Fig. 2 is the ultra-fine acetate fiber prepared using the embodiment of the present invention 5
Plain nanofiber growth in situ MnO2The scanning electron microscope schematic diagram of adsorbent.10mg adsorbent obtained above is taken, is added to
30mL concentration is the Pb of 100mg/L2+Adsorption liquid；Adsorption temp is 25 DEG C；Adsorption time is for 24 hours；Adsorption liquid pH value is 6.Absorption
After the completion, using in icp ms (ICP, Varian 715-ES, Varian company, the U.S.) test solution
Remaining Pb2+Concentration, obtain the adsorbent to Pb2+Adsorbance be 234.3mg/g.
Claims (1)
1. a kind of preparation method of the efficient adsorbents for lead ion pyrolytic of growth in situ manganese dioxide characterized by comprising
(1) configuration of spinning solution: a certain amount of redox graphene powder is added to containing a certain amount of four hexyls ammonium bromide
In high polymeric solution, ultrasonic disperse 0.5h obtains electrostatic spinning liquid；
The high polymer is cellulose acetate, nylon 6；
The high polymeric solution concentration is 8~20%；
It is 0.1~0.3% that the redox graphene, which accounts for the polymer dope mass percent,；
The four hexyl bromination ammonium concentrations are 0.05~0.15mol L-1；
(2) electrostatic spinning: by previous step spinning solution using method of electrostatic spinning carry out spinning, at room temperature, relative humidity be 20 ±
10%, spinning voltage is 15~35kV, and receiving distance is 10~20cm, and feed flow rate is 0.5~1.5mL/h, and oxygen reduction is made
Graphite alkene adulterates ultra-fine polymer nano fibrous membrane；
(3) growth in situ manganese dioxide: a certain amount of potassium permanganate is dissolved into deionized water, tunica fibrosa prepared by previous step
It takes out, is added in liquor potassic permanganate；It is added dropwise into above-mentioned solution after 1h is stirred at room temperature in a certain amount of concentrated sulfuric acid, by above-mentioned mixing
Object is transferred to hydrothermal reaction kettle, 60 DEG C of reaction 6h, and reaction terminates, and tunica fibrosa taking-up deionized water repeated flushing is dried, system
Obtain growth in situ manganese dioxide adsorbents for lead ion pyrolytic；
The mass fraction 0.01~0.1% of the liquor potassic permanganate；
The mass percent that the concentrated sulfuric acid accounts for the liquor potassic permanganate is 1~3%.
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Cited By (5)
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|---|---|---|---|---|
| CN110075785A (en) * | 2019-05-08 | 2019-08-02 | 河南城建学院 | The MnO of lead ion in a kind of removing water2Composite material and preparation method |
| CN111135802A (en) * | 2020-01-19 | 2020-05-12 | 浙江大学 | Preparation method for constructing water treatment biomembrane by modifying manganese dioxide particles with silk fibroin planar wires |
| CN111422977A (en) * | 2020-01-19 | 2020-07-17 | 浙江大学 | Preparation method for constructing multilayer duplex-structure water treatment biological membrane by taking silkworm plane silk as substrate |
| CN113976088A (en) * | 2021-11-30 | 2022-01-28 | 广东石油化工学院 | Preparation method of polyamide 6/graphene oxide/iron-based metal organic framework three-phase composite material |
| CN116328712A (en) * | 2023-03-15 | 2023-06-27 | 中国舰船研究设计中心 | Novel water quality purifying composite material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110075785A (en) * | 2019-05-08 | 2019-08-02 | 河南城建学院 | The MnO of lead ion in a kind of removing water2Composite material and preparation method |
| CN111135802A (en) * | 2020-01-19 | 2020-05-12 | 浙江大学 | Preparation method for constructing water treatment biomembrane by modifying manganese dioxide particles with silk fibroin planar wires |
| CN111422977A (en) * | 2020-01-19 | 2020-07-17 | 浙江大学 | Preparation method for constructing multilayer duplex-structure water treatment biological membrane by taking silkworm plane silk as substrate |
| CN111422977B (en) * | 2020-01-19 | 2021-10-01 | 浙江大学 | Preparation method for constructing multilayer duplex-structure water treatment biological membrane by taking silkworm plane silk as substrate |
| CN113976088A (en) * | 2021-11-30 | 2022-01-28 | 广东石油化工学院 | Preparation method of polyamide 6/graphene oxide/iron-based metal organic framework three-phase composite material |
| CN116328712A (en) * | 2023-03-15 | 2023-06-27 | 中国舰船研究设计中心 | Novel water quality purifying composite material and preparation method and application thereof |
| CN116328712B (en) * | 2023-03-15 | 2024-04-16 | 中国舰船研究设计中心 | Novel water quality purifying composite material and preparation method and application thereof |
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