CN108246258A - A kind of preparation method of magnetism aminated carbon nano tube - Google Patents

A kind of preparation method of magnetism aminated carbon nano tube Download PDF

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Publication number
CN108246258A
CN108246258A CN201810083587.5A CN201810083587A CN108246258A CN 108246258 A CN108246258 A CN 108246258A CN 201810083587 A CN201810083587 A CN 201810083587A CN 108246258 A CN108246258 A CN 108246258A
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magnetic
carbon nano
preparation
carbon nanotube
tube
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CN201810083587.5A
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Chinese (zh)
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杨立业
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Zhejiang Ocean University ZJOU
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Zhejiang Ocean University ZJOU
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Priority to CN201810083587.5A priority Critical patent/CN108246258A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B01J20/205Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28009Magnetic properties
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/283Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/48Treatment of water, waste water, or sewage with magnetic or electric fields
    • C02F1/488Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/36Organic compounds containing halogen

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Inorganic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

A kind of preparation method of magnetism aminated carbon nano tube, the preparation method are:Magnetic carbon nano-tube is prepared by coprecipitation first, then modifies to obtain more amino by polyethylene ammonia, obtains magnetic aminated carbon nano tube;The method that the coprecipitation prepares magnetic carbon nano-tube is:Using aqueous reaction coprecipitation, the modification of carbon nanotube is carried out with Fe3O4@SiO2 magnetic nano-particles, the magnetic multi-walled carbon nanotube of ferroso-ferric oxide modification is made;The method that the polyethylene ammonia is modified to obtain magnetic aminated carbon nano tube is:To be immersed in the mixed solution containing ethyl alcohol, water and polyethylene ammonia after magnetic multi-walled carbon nanotube high-temperature process, after impregnating at room temperature, washing, drying obtain amidized magnetic multi-walled carbon nanotube;The present invention is simple with preparation process, and using the prior art, preparation can carry out absorption removal to diclofenac in water, reach the features such as fast and easy persistently removes effect.

Description

A kind of preparation method of magnetism aminated carbon nano tube
Technical field
The present invention relates to a kind of preparation method of magnetic aminated carbon nano tube, in particular for double chlorine in absorption water The preparation method of the magnetic aminated carbon nano tube of phenolic acid sodium belongs to the technical field of adsorption material preparation of water process.
Background technology
Diclofenac is the common medicine of human lives as rheumatoid and osteoarthritis medicine;It is also PPCPs (drugs One of and personal care articles), to human health, there are certain hidden danger, how quickly to carry out absorption shifting to diclofenac in water Except as current urgent problem.
There is a kind of magnetic microsphere of common absorption diclofenac in the prior art, such as 201710814222.0 inventions are special Profit application;But the effect of existing these magnetic microspheres absorption diclofenac is not very ideal, without sustainable absorption Performance.
Invention content
It is an object of the invention to overcome the shortcomings of the prior art, and it is simple to provide a kind of preparation process, using existing There is technology, preparation can carry out absorption removal to diclofenac in water, reach the magnetic ammonia that fast and easy persistently removes effect The preparation method of base carbon nano tube.
The purpose of the present invention is by following technical solution to complete, a kind of preparation side of magnetism aminated carbon nano tube Method, the preparation method are:Magnetic carbon nano-tube is prepared by coprecipitation first, then modifies to obtain by polyethylene ammonia More amino obtain magnetic aminated carbon nano tube.
As preferred:The method that the coprecipitation prepares magnetic carbon nano-tube is:Using aqueous reaction coprecipitation, The modification of carbon nanotube is carried out with Fe3O4@SiO2 magnetic nano-particles, the magnetic multi-wall carbon nano-tube of ferroso-ferric oxide modification is made Pipe;
The method that the polyethylene ammonia is modified to obtain magnetic aminated carbon nano tube is:At magnetic multi-walled carbon nanotube high temperature After reason immerse the mixed solution containing ethyl alcohol, water and polyethylene ammonia in, at room temperature impregnate after, washing, drying obtain it is amidized Magnetic multi-walled carbon nanotube.
As preferred:The magnetism multi-walled carbon nanotube high-temperature process is in 300-350 DEG C, 2-5 hours time;It is described Ratio in the mixed solution of ethyl alcohol, water and polyethylene ammonia is:1:1:0.05—0.2;At room temperature soaking time for 12-for 24 hours; 60-80 DEG C of drying temperature, the time 12-for 24 hours.
The present invention can be utilized to be studied based on diclofenac in multi-walled carbon nanotube absorption sanitary sewage, and research obtains most Good adsorption conditions after material completes absorption, carry out it Magneto separate processing, and carry out elution cycles utilization, can reduce sewage Middle diclofenac content, and the utilization rate of material can be improved;Processing for PPCPs in sanitary sewage provides a kind of new think of Road.
The present invention is simple with preparation process, and using the prior art, preparation can adsorb diclofenac in water It removes, reaches the features such as fast and easy persistently removes effect.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail:A kind of magnetic amination carbon of the present invention The preparation method of nanotube, the preparation method are:Magnetic carbon nano-tube is prepared by coprecipitation first, then by poly- Ethylene ammonia is modified to obtain more amino, obtains magnetic aminated carbon nano tube.
The preferred embodiment of the invention is:The method that the coprecipitation prepares magnetic carbon nano-tube is:Using water phase Chemical coprecipitation carries out the modification of carbon nanotube with Fe3O4@SiO2 magnetic nano-particles, and ferroso-ferric oxide modification is made Magnetic multi-walled carbon nanotube;
The method that the polyethylene ammonia is modified to obtain magnetic aminated carbon nano tube is:At magnetic multi-walled carbon nanotube high temperature After reason immerse the mixed solution containing ethyl alcohol, water and polyethylene ammonia in, at room temperature impregnate after, washing, drying obtain it is amidized Magnetic multi-walled carbon nanotube.
As further preferred embodiment, magnetism multi-walled carbon nanotube high-temperature process of the present invention is 300-350 DEG C, 2-5 hours time;Ratio in the mixed solution of the ethyl alcohol, water and polyethylene ammonia is:1:1:0.05—0.2;Room temperature Lower soaking time for 12-for 24 hours;60-80 DEG C of drying temperature, the time 12-for 24 hours.
Multi-walled carbon nanotube of the present invention is the nano material for having good adsorption properties, has huge specific surface Product, it prepares magnetic carbon nano-tube by coprecipitation first, then modifies to obtain more amino by polyethylene ammonia.
Have it is many research shows that, carbon nanotube is huge to many pollutants good absorption property, but here by magnetic Carbon nanotube after sex modification again modify by amination, the carry out adsorbing separation of more convenient and quicker, and passes through adsorption capacity and removal Rate compares document, and it is an absorption property sustainable adsorbent very well that can find this.

Claims (3)

1. a kind of preparation method of magnetism aminated carbon nano tube, it is characterised in that the preparation method is:First by altogether The precipitation method prepare magnetic carbon nano-tube, then modify to obtain more amino by polyethylene ammonia, obtain magnetic amination carbon and receive Mitron.
2. the preparation method of magnetism aminated carbon nano tube according to claim 1, it is characterised in that the co-precipitation The method that method prepares magnetic carbon nano-tube is:Using aqueous reaction coprecipitation, carried out with Fe3O4@SiO2 magnetic nano-particles The magnetic multi-walled carbon nanotube of ferroso-ferric oxide modification is made in the modification of carbon nanotube;
The method that the polyethylene ammonia is modified to obtain magnetic aminated carbon nano tube is:At magnetic multi-walled carbon nanotube high temperature After reason immerse the mixed solution containing ethyl alcohol, water and polyethylene ammonia in, at room temperature impregnate after, washing, drying obtain it is amidized Magnetic multi-walled carbon nanotube.
3. the preparation method of magnetism aminated carbon nano tube according to claim 2, it is characterised in that the magnetism multi wall Carbon nanotube high-temperature process is in 300-350 DEG C, 2-5 hours time;In the mixed solution of the ethyl alcohol, water and polyethylene ammonia Ratio be:1:1:0.05—0.2;At room temperature soaking time for 12-for 24 hours;60-80 DEG C of drying temperature, the time 12-for 24 hours.
CN201810083587.5A 2018-01-29 2018-01-29 A kind of preparation method of magnetism aminated carbon nano tube Pending CN108246258A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109550480A (en) * 2018-11-23 2019-04-02 浙江海洋大学 A kind of preparation method of amination magnetic carbon nano-tube
CN110204063A (en) * 2019-06-04 2019-09-06 成都纳海川环境工程有限公司 The preparation method of heavy passenger's motortruck engine water circulation inorganic particle scale dispersing agent
CN114229913A (en) * 2021-12-21 2022-03-25 华南理工大学 Nano ferroferric oxide/aminated carbon nanotube composite material based on hydrogen bonding and preparation method thereof

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20050107094A (en) * 2004-05-07 2005-11-11 한국과학기술원 Method for carbon nanotubes array using magnetic material
CN102391831A (en) * 2011-12-07 2012-03-28 复旦大学 Carbon nanotube composite material modified by magnetic nanoparticles, its preparation method and application
CN102553526A (en) * 2011-12-20 2012-07-11 华北电力大学(保定) Method for removing mercury ions from water by using silver-modified magnetic carbon nanotube and regeneration method
CN105129898A (en) * 2015-08-26 2015-12-09 宁波大学 Renewable amino functionalized magnetic carbon nano composite material, and preparation method therefor and application thereof
CN106475042A (en) * 2016-11-30 2017-03-08 吉林化工学院 A kind of magnetic Nano material Fe of absorbing dye methylene blue3O4@SiO2The preparation method of@MWNTs
CN106732470A (en) * 2017-03-06 2017-05-31 济南大学 A kind of preparation of 2 mercaptopyrimidine modified magnetic CNT porous adsorbent
CN107570116A (en) * 2017-09-27 2018-01-12 浙江海洋大学 The magnetic MOFs sorbing materials of antibiotic in a kind of adsorbed water body
CN107583617A (en) * 2017-09-11 2018-01-16 浙江海洋大学 A kind of magnetic microsphere for adsorbing diclofenac

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20050107094A (en) * 2004-05-07 2005-11-11 한국과학기술원 Method for carbon nanotubes array using magnetic material
CN102391831A (en) * 2011-12-07 2012-03-28 复旦大学 Carbon nanotube composite material modified by magnetic nanoparticles, its preparation method and application
CN102553526A (en) * 2011-12-20 2012-07-11 华北电力大学(保定) Method for removing mercury ions from water by using silver-modified magnetic carbon nanotube and regeneration method
CN105129898A (en) * 2015-08-26 2015-12-09 宁波大学 Renewable amino functionalized magnetic carbon nano composite material, and preparation method therefor and application thereof
CN106475042A (en) * 2016-11-30 2017-03-08 吉林化工学院 A kind of magnetic Nano material Fe of absorbing dye methylene blue3O4@SiO2The preparation method of@MWNTs
CN106732470A (en) * 2017-03-06 2017-05-31 济南大学 A kind of preparation of 2 mercaptopyrimidine modified magnetic CNT porous adsorbent
CN107583617A (en) * 2017-09-11 2018-01-16 浙江海洋大学 A kind of magnetic microsphere for adsorbing diclofenac
CN107570116A (en) * 2017-09-27 2018-01-12 浙江海洋大学 The magnetic MOFs sorbing materials of antibiotic in a kind of adsorbed water body

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109550480A (en) * 2018-11-23 2019-04-02 浙江海洋大学 A kind of preparation method of amination magnetic carbon nano-tube
CN109550480B (en) * 2018-11-23 2022-01-11 浙江海洋大学 Preparation method of aminated magnetic carbon nanotube
CN110204063A (en) * 2019-06-04 2019-09-06 成都纳海川环境工程有限公司 The preparation method of heavy passenger's motortruck engine water circulation inorganic particle scale dispersing agent
CN114229913A (en) * 2021-12-21 2022-03-25 华南理工大学 Nano ferroferric oxide/aminated carbon nanotube composite material based on hydrogen bonding and preparation method thereof
CN114229913B (en) * 2021-12-21 2022-09-20 华南理工大学 Nano ferroferric oxide/aminated carbon nanotube composite material based on hydrogen bonding and preparation method thereof

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