CN107670640A - Immobilized quaternary ammonium salt magnetic functional material of CNT and its preparation method and application - Google Patents
Immobilized quaternary ammonium salt magnetic functional material of CNT and its preparation method and application Download PDFInfo
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- CN107670640A CN107670640A CN201710969535.3A CN201710969535A CN107670640A CN 107670640 A CN107670640 A CN 107670640A CN 201710969535 A CN201710969535 A CN 201710969535A CN 107670640 A CN107670640 A CN 107670640A
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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
- B01J20/20—Solid 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
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid 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
- B01J20/28009—Magnetic properties
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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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F2101/12—Halogens or halogen-containing compounds
Abstract
The present invention relates to immobilized quaternary ammonium salt magnetic functional material of a kind of CNT and its preparation method and application, it is characterised in that：The immobilized quaternary ammonium salt magnetic functional material of CNT includes carboxylic carbon nano-tube, it is coated on the nano magnetic material on the carboxylic carbon nano-tube surface, the amination reagent on the carboxylic carbon nano-tube surface is immobilized on, and the quaternary ammonium salt functional reagent being grafted on amination reagent.Compared with prior art, the advantage of the invention is that：The perchlorate that the obtained immobilized quaternary ammonium salt magnetic functional material of CNT can be applied in water removal, its relatively high magnetism, has higher adsorption capacity and preferable adsorptive selectivity；And preparation method is simple.
Description
Technical field
The invention belongs to water prevention and cure of pollution field of functional materials, and in particular to a kind of immobilized quaternary ammonium salt magnetic of CNT
Functional material and its preparation method and application
Background technology
For perchlorate as a kind of emerging pollutant of the persistence with high diffusion, taking in can be with iodide ion after human body
Competition enters thyroid gland, induces thyroid cancer, and therefore, perchlorate is also known as " strength thyroidotoxin ".Fireworks, explosive etc. are solid
In the production process of body propellant, ammonium perchlorate is widely used as oxidant, and a small amount of ammonium perchlorate can pass through medium
Water penetration is migrated to surface and ground water, and its pollution situation to water body is by extensive concern both domestic and external.From 1997 with
Come, USEPA successively detects perchlorate in the underground water, surface water and drinking water in 42 states such as California.Therefore, to water body
The control research of middle perchlorate turns into water process and the study hotspot in water prevention and cure of pollution field.
In recent years, have scholar by the use of CNT as adsorbent go water removal in remain perchlorate (Q.Fang,
B.Chen,Adsorption of perchlorate onto raw and oxidized carbon nanotubes in
aqueous solution.Carbon,2012,50,2209).Although CNT can be to remain perchloric acid in efficient absorption water
Salt, but remain be not easy to realize separation of solid and liquid, power of regeneration difference the deficiencies of.In addition, CNT is in absorption perchlorate
The inorganic anion such as adsorbable bromate, nitrate, nitrite and iodate simultaneously, the absorption selection for perchlorate
Poor (F.Metzelder, T.C.Schmidt, Environmental conditions the influencing sorption of property
of inorganic anions to multiwalled carbon nanotubes studied by column
chromatography.Environmental Science Technology,2017,51,4928).There is scholar to use quaternary ammonium
Salt greatly improves adsorptive selectivity of the adsorbent to perchlorate as adsorption function base group modification giantreed and activated carbon.Mirror
High selectivity in CNT to the strong adsorption capacity of perchlorate and quaternary ammonium salt functional group to perchlorate, therefore open
A kind of functional material of combination CNT and quaternary ammonium salt is sent to come before the perchlorate in adsorbed water body has a wide range of applications
Scape, and not yet occur such material in the prior art.
The content of the invention
First technical problem to be solved by this invention is the present situation for prior art, there is provided a kind of adsorption capacity
Greatly, selective adsorption capacity is strong, the immobilized quaternary ammonium salt magnetic functional material of CNT of separation of solid and liquid can be achieved.
Second technical problem to be solved by this invention is the present situation for prior art, there is provided a kind of above-mentioned carbon nanometer
Manage the preparation method of immobilized quaternary ammonium salt magnetic functional material.
3rd technical problem to be solved by this invention is the present situation for prior art, there is provided one kind utilizes above-mentioned carbon
The immobilized quaternary ammonium salt magnetic functional material of nanotube goes the application of perchlorate in water removal.
Technical scheme is used by the present invention solves above-mentioned first technical problem：A kind of immobilized quaternary ammonium salt of CNT
Magnetic functional material, it is characterised in that：Including carboxylic carbon nano-tube, the nanometer on the carboxylic carbon nano-tube surface is coated on
Magnetic material, it is immobilized on the amination reagent on the carboxylic carbon nano-tube surface, and the quaternary ammonium being grafted on amination reagent
Salt functional reagent.
In such scheme, the nano magnetic material is nano ferriferrous oxide.
As an improvement, the amination reagent is diethylenetriamine.
Improve, the quaternary ammonium salt functional reagent is 2,3- epoxypropyltrimethylchloride chlorides, 2,3- glycidyl triethyl groups
At least one of ammonium chloride.
Technical scheme is used by the present invention solves above-mentioned second technical problem：A kind of above-mentioned CNT immobilized season
The preparation method of ammonium salt magnetic functional material, it is characterised in that comprise the following steps：
(1) the immobilized amino-magnetic functional material of CNT is prepared using solvent-thermal method：By 0.5~3.0g FeCl3·
6H2O is added into 20mL ethylene glycol, and ultrasonic disperse is limpid to solution；Then add 3.0g anhydrous sodium acetates, 0.5~5mL ammoniacal liquor
Solution and 5~20mL amination reagent, 20~100mg carboxylic carbon nano-tube, 5~10min of ultrasonic disperse then will be mixed
Close solution and add into polytetrafluoroethylene (PTFE) autoclave and react 5~12h in 160~250 DEG C, be cooled to room temperature, Magneto separate, use is ultrapure
Water washing is washed for several times to acid-base value in neutrality, then with ethanol for several times, 30~90 DEG C of 6~12h of vacuum drying, CNT is made
Immobilized amino-magnetic functional material.
(2) the immobilized quaternary ammonium salt magnetic functional material of CNT is prepared using ring-opening reaction：Carbon prepared by step (1) is received
0.5~2.5g of the immobilized amino-magnetic functional material of mitron is added into 50mL methanol, 5~10min of ultrasonic disperse to being uniformly dispersed,
60~90 DEG C are warming up to, 2~10mL quaternary ammonium salt functional reagents, 6~12h of back flow reaction is added dropwise.It is cooled to room temperature, magnetic point
From, it is in for several times neutrality to acid-base value with milli-Q water, then washed for several times with ethanol, 30~90 DEG C of 6~12h of vacuum drying, make
Obtain the immobilized quaternary ammonium salt magnetic functional material of CNT.
Preferably, in the step (1) ammonia spirit be content be 10% (V/V) and 25% (V/V) ammoniacal liquor in extremely
Few one kind.
Technical scheme is used by the present invention solves above-mentioned 3rd technical problem：A kind of above-mentioned CNT immobilized season
The application of ammonium salt magnetic functional material, it is characterised in that：20~100mg of the immobilized quaternary ammonium salt magnetic functional material of CNT is added
To 100mL, concentration is in 5.0~500mg/L perchlorate solution, adjusts pH to 2~9, then constant temperature shakes at 15~50 DEG C
1~120min is swung, that is, completes the application that the immobilized quaternary ammonium salt magnetic functional material of CNT removes perchlorate in water removal.
Compared with prior art, the advantage of the invention is that：
(1) relatively high magnetism, the immobilized quaternary ammonium salt magnetic functional material of CNT produced by the present invention have superparamagnetism, energy
That enough stablizes in the solution is scattered, can realize that quick separation of solid and liquid is enriched with using simple magnetic fields.
(2) preparation method is simple, and the immobilized quaternary ammonium salt magnetic function of CNT is obtained using solvent-thermal method and ring-opening reaction
Material, a kind of strong basicity reaction environment is provided by ammoniacal liquor, generated in-situ nano ferriferrous oxide is uniformly coated on carbon
Nanotube surface, while amination reagent is immobilized on carbon nano tube surface through acylation reaction；By ring-opening reaction by quaternary ammonium salt
Activity functional groups are grafted on acylated amination reagent；The immobilized quaternary ammonium salt magnetic function material of CNT produced by the present invention
Expect due to the carboxyl on carboxylic carbon nano-tube surface and the amido in amination reagent and the amido and quaternary ammonium of amination reagent
Chemical bonding effect between salt functional reagent epoxy group, adhesion is stronger, and property is stable, and prepared CNT is immobilized
Nano ferriferrous oxide homogeneous grain diameter in quaternary ammonium salt magnetic functional material, and its pattern is spherical.
(3) present invention passes through the controllable preparation of the immobilized quaternary ammonium salt magnetic functional material of CNT, absorption pH, absorption temperature
The optimization of the conditions such as degree, adsorption time, perchlorate concentration, the immobilized quaternary ammonium salt magnetic functional material of CNT can be made to water
Middle perchlorate has powerful removal ability, so that the immobilized quaternary ammonium salt magnetic functional material of CNT is applied to water environment
The elimination of middle perchlorate；Meanwhile saved processing time and cost, with existing CNT, quaternary ammonium salt modification activities charcoal,
The sorbing materials such as quaternary ammonium salt modification giantreed, which are compared in terms of perchlorate removal, has higher adsorption capacity and preferably absorption
Selectivity.
Brief description of the drawings
Fig. 1 is the projection electron microscope of the immobilized quaternary ammonium salt magnetic functional material of CNT of the embodiment of the present invention one；
Fig. 2 is the hysteresis curve figure of the immobilized quaternary ammonium salt magnetic functional material of CNT of the embodiment of the present invention one；
Fig. 3 is the x-ray photoelectron power spectrum of the immobilized quaternary ammonium salt magnetic functional material of CNT of the embodiment of the present invention one
Figure.
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.
Embodiment one：
A kind of preparation method of the immobilized quaternary ammonium salt magnetic functional material of CNT, comprises the following steps：
(1) the immobilized amino-magnetic functional material of CNT is prepared using solvent-thermal method, by 2.0g FeCl3·6H2O is added
Into 20mL ethylene glycol, ultrasonic disperse is limpid to solution；3.0g anhydrous sodium acetates are then added, add 0.5mL, concentration is
10% (V/V) ammonia spirit, 20mL diethylenetriamines and 50mg carboxylic carbon nano-tubes, ultrasonic disperse 10min then will be above-mentioned
Mixed solution is added into polytetrafluoroethylene (PTFE) autoclave reacts 10h in 200 DEG C.Room temperature is cooled to, Magneto separate, uses milli-Q water
It is for several times 7.0 to pH, then is washed for several times with ethanol, 60 DEG C of vacuum drying 6h, the immobilized amino-magnetic function material of CNT is made
Material.
(2) the immobilized quaternary ammonium salt magnetic functional material of CNT is prepared using ring-opening reaction, carbon prepared by step (1) is received
The immobilized amino-magnetic functional material 1.0g of mitron is added into 50mL methanol, and ultrasonic disperse 10min is warming up to 80 to being uniformly dispersed
DEG C, it is added dropwise 2mL 2,3- epoxypropyltrimethylchloride chlorides, back flow reaction 8h is cooled to room temperature, Magneto separate, and use is ultrapure
Water washing is for several times 7.0 to pH, then is washed for several times with ethanol, 60 DEG C of vacuum drying 6h, the immobilized quaternary ammonium salt magnetic of CNT is made
Sexual function material.
The transmission electron microscope picture of the obtained immobilized quaternary ammonium salt magnetic functional material of CNT is as shown in figure 1, CNT is consolidated
Carry Fe in quaternary ammonium salt magnetic functional material3O4Particle diameter is 50nm, its pattern rule, uniform particle diameter, is evenly distributed on CNT table
Face.The immobilized quaternary ammonium salt magnetic functional material of obtained CNT has strong saturation magnetization (72.2emu/ as seen from Figure 2
G), it is made to realize efficient displacement under external magnetic field and then beneficial to the recovery use of material.As shown in figure 3, carbon is received
Carbon spectrum (C 1s), the bonded energy of oxygen spectrum (O 1s) and nitrogen spectrum (N 1s) are respectively in the immobilized quaternary ammonium salt magnetic functional material of mitron
284.0eV, 530.2eV and 399.8eV, show that quaternary ammonium salt activity functional groups are successfully immobilized on magnetic carbon nano-tube surface.
The immobilized quaternary ammonium salt magnetic functional material 50mg of CNT obtained above is added to 100mL, concentration is
In 100mg/L perchlorate solution, pH to 3 is adjusted, then the constant temperature oscillation 10min at 30 DEG C, that is, complete CNT and consolidate
Carry the application that quaternary ammonium salt magnetic functional material removes perchlorate in water removal.The immobilized quaternary ammonium salt magnetic functional material absorption of CNT
The adsorbance of perchlorate is 70mg/g in water.
Embodiment two：
A kind of preparation method of the immobilized quaternary ammonium salt magnetic functional material of CNT, comprises the following steps：
(1) the immobilized amino-magnetic functional material of CNT is prepared using solvent-thermal method, by 2.0g FeCl3·6H2O is added
Into 20mL ethylene glycol, ultrasonic disperse is limpid to solution；3.0g anhydrous sodium acetates are then added, adding 2.0mL concentration is
25% (V/V) ammonia spirit, 10mL diethylenetriamines and 100mg carboxylic carbon nano-tubes, ultrasonic disperse 8min then will mixing
Solution is added into polytetrafluoroethylene (PTFE) autoclave reacts 12h in 200 DEG C.It is cooled to room temperature, Magneto separate, with milli-Q water for several times
It is 7.0 to pH, then is washed for several times with ethanol, 30 DEG C of vacuum drying 12h, the immobilized amino-magnetic functional material of CNT is made.
(2) the immobilized quaternary ammonium salt magnetic functional material of CNT is prepared using ring-opening reaction, carbon prepared by step (1) is received
The immobilized amino-magnetic functional material 2.5g of mitron is added into 50mL methanol, and ultrasonic disperse 5min is warming up to 80 to being uniformly dispersed
DEG C, 10mL 2,3- Epoxypropyl triethyl ammonium chloride agent, back flow reaction 12h is added dropwise.Room temperature is cooled to, Magneto separate, is used
Milli-Q water is for several times 7.0 to pH, then is washed for several times with ethanol, 30 DEG C of vacuum drying 12h, the immobilized quaternary ammonium of CNT is made
Salt magnetic functional material.
The immobilized quaternary ammonium salt magnetic functional material 100mg of CNT obtained above is added to 100mL, concentration is
In 400mg/L perchlorate solution, pH to 9 is adjusted, then the constant temperature oscillation 100min at 50 DEG C, that is, complete CNT and consolidate
Carry the application that quaternary ammonium salt magnetic functional material removes perchlorate in water removal.The immobilized quaternary ammonium salt magnetic functional material absorption of CNT
The adsorbance of perchlorate is 152mg/g in water.
Embodiment three：
A kind of preparation method of the immobilized quaternary ammonium salt magnetic functional material of CNT, comprises the following steps：
(1) the immobilized amino-magnetic functional material of CNT is prepared using solvent-thermal method, by 2.0g FeCl3·6H2O is added
Into 20mL ethylene glycol, ultrasonic disperse is limpid to solution；3.0g anhydrous sodium acetates are then added, add 5mL, concentration 10%
(V/V) ammonia spirit, 5mL diethylenetriamines and 20mg carboxylic carbon nano-tubes, ultrasonic disperse 5min are then molten by above-mentioned mixing
Liquid is added into polytetrafluoroethylene (PTFE) autoclave reacts 5h in 200 DEG C.It is cooled to room temperature, Magneto separate, with milli-Q water for several times extremely
PH is 7.0, then is washed for several times with ethanol, 90 DEG C of vacuum drying 8h, the immobilized amino-magnetic functional material of CNT is made.
(2) the immobilized quaternary ammonium salt magnetic functional material of CNT is prepared using ring-opening reaction, carbon prepared by step (1) is received
The immobilized amino-magnetic functional material 0.5g of mitron is added into 50mL methanol, and ultrasonic disperse 8min is warming up to 80 to being uniformly dispersed
DEG C, it is added dropwise 5mL 2,3- epoxypropyltrimethylchloride chlorides, back flow reaction 6h is cooled to room temperature, Magneto separate, and use is ultrapure
Water washing is for several times 7.0 to pH, then is washed for several times with ethanol, 90 DEG C of vacuum drying 8h, the immobilized quaternary ammonium salt magnetic of CNT is made
Sexual function material.
The immobilized quaternary ammonium salt magnetic functional material 20mg of CNT obtained above is added to 100mL, concentration 5mg/L
Perchlorate solution in, adjust pH to 6, then the constant temperature oscillation 1min at 15 DEG C, that is, complete the immobilized quaternary ammonium salt of CNT
Magnetic functional material goes the application of perchlorate in water removal.High chlorine in the immobilized quaternary ammonium salt magnetic functional material absorption water of CNT
The adsorbance of hydrochlorate is 122mg/g.
Example IV：
(1) the immobilized amino-magnetic functional material of CNT is prepared using solvent-thermal method, by 0.5g FeCl3·6H2O is added
Into 20mL ethylene glycol, ultrasonic disperse is limpid to solution；3.0g anhydrous sodium acetates are then added, add 0.5mL, concentration is
10% (V/V) ammonia spirit, 20mL diethylenetriamines and 50mg carboxylic carbon nano-tubes, ultrasonic disperse 10min then will be above-mentioned
Mixed solution is added into polytetrafluoroethylene (PTFE) autoclave reacts 10h in 160 DEG C.Room temperature is cooled to, Magneto separate, uses milli-Q water
It is for several times 7.0 to pH, then is washed for several times with ethanol, 60 DEG C of vacuum drying 6h, the immobilized amino-magnetic function material of CNT is made
Material.
(2) the immobilized quaternary ammonium salt magnetic functional material of CNT is prepared using ring-opening reaction, carbon prepared by step (1) is received
The immobilized amino-magnetic functional material 1.0g of mitron is added into 50mL methanol, and ultrasonic disperse 10min is warming up to 60 to being uniformly dispersed
DEG C, it is added dropwise 2mL 2,3- epoxypropyltrimethylchloride chlorides, back flow reaction 8h is cooled to room temperature, Magneto separate, and use is ultrapure
Water washing is for several times 7.0 to pH, then is washed for several times with ethanol, 60 DEG C of vacuum drying 6h, the immobilized quaternary ammonium salt magnetic of CNT is made
Sexual function material.
The immobilized quaternary ammonium salt magnetic functional material 50mg of CNT obtained above is added to 100mL, concentration is
In 100mg/L perchlorate solution, pH to 3 is adjusted, then the constant temperature oscillation 10min at 30 DEG C, that is, complete CNT and consolidate
Carry the application that quaternary ammonium salt magnetic functional material removes perchlorate in water removal.The immobilized quaternary ammonium salt magnetic functional material absorption of CNT
The adsorbance of perchlorate is 86.2mg/g in water.
Embodiment five：
(1) the immobilized amino-magnetic functional material of CNT is prepared using solvent-thermal method, by 3.0g FeCl3·6H2O is added
Into 20mL ethylene glycol, ultrasonic disperse is limpid to solution；3.0g anhydrous sodium acetates are then added, add 0.5mL, concentration is
10% (V/V) ammonia spirit, 20mL diethylenetriamines and 50mg carboxylic carbon nano-tubes, ultrasonic disperse 10min then will be above-mentioned
Mixed solution is added into polytetrafluoroethylene (PTFE) autoclave reacts 10h in 250 DEG C.Room temperature is cooled to, Magneto separate, uses milli-Q water
It is for several times 7.0 to pH, then is washed for several times with ethanol, 60 DEG C of vacuum drying 6h, the immobilized amino-magnetic function material of CNT is made
Material.
(2) the immobilized quaternary ammonium salt magnetic functional material of CNT is prepared using ring-opening reaction, carbon prepared by step (1) is received
The immobilized amino-magnetic functional material 1.0g of mitron is added into 50mL methanol, and ultrasonic disperse 10min is warming up to 90 to being uniformly dispersed
DEG C, it is added dropwise 2mL 2,3- epoxypropyltrimethylchloride chlorides, back flow reaction 8h is cooled to room temperature, Magneto separate, and use is ultrapure
Water washing is for several times 7.0 to pH, then is washed for several times with ethanol, 60 DEG C of vacuum drying 6h, the immobilized quaternary ammonium salt magnetic of CNT is made
Sexual function material.
The immobilized quaternary ammonium salt magnetic functional material 50mg of CNT obtained above is added to 100mL, concentration is
In 100mg/L perchlorate solution, pH to 3 is adjusted, then the constant temperature oscillation 10min at 30 DEG C, that is, complete CNT and consolidate
Carry the application that quaternary ammonium salt magnetic functional material removes perchlorate in water removal.The immobilized quaternary ammonium salt magnetic functional material absorption of CNT
The adsorbance of perchlorate is 52.8mg/g in water.
Claims (7)
- A kind of 1. immobilized quaternary ammonium salt magnetic functional material of CNT, it is characterised in that：Including carboxylic carbon nano-tube, it is coated on The nano magnetic material on the carboxylic carbon nano-tube surface, it is immobilized on the amination examination on the carboxylic carbon nano-tube surface Agent, and the quaternary ammonium salt functional reagent being grafted on amination reagent.
- 2. the immobilized quaternary ammonium salt magnetic functional material of CNT according to claim 1, it is characterised in that：The nano magnetic Property material is nano ferriferrous oxide.
- 3. the immobilized quaternary ammonium salt magnetic functional material of CNT according to claim 1, it is characterised in that：The amination Reagent is diethylenetriamine.
- 4. the immobilized quaternary ammonium salt magnetic functional material of CNT according to claim 1, it is characterised in that：The quaternary ammonium salt Functional reagent is at least one of 2,3- epoxypropyltrimethylchloride chlorides, 2,3- Epoxypropyl triethyl ammonium chlorides.
- A kind of 5. preparation side of the immobilized quaternary ammonium salt magnetic functional material of CNT as described in any claim of Claims 1 to 4 Method, it is characterised in that comprise the following steps：(1) the immobilized amino-magnetic functional material of CNT is prepared using solvent-thermal method：By 0.5~3.0g FeCl3·6H2O adds Enter into 20mL ethylene glycol, ultrasonic disperse is limpid to solution；Then add 3.0g anhydrous sodium acetates, 0.5~5mL ammonia spirits and 5~20mL amination reagent, 20~100mg carboxylic carbon nano-tube, 5~10min of ultrasonic disperse, then by above-mentioned mixing Solution is added into polytetrafluoroethylene (PTFE) autoclave reacts 5~12h in 160~250 DEG C, is cooled to room temperature, Magneto separate, uses ultra-pure water Washing is washed for several times to acid-base value in neutrality, then with ethanol for several times, and 30~90 DEG C of 6~12h of vacuum drying, obtained CNT is consolidated Carry amino-magnetic functional material.(2) the immobilized quaternary ammonium salt magnetic functional material of CNT is prepared using ring-opening reaction：CNT prepared by step (1) 0.5~2.5g of immobilized amino-magnetic functional material is added into 50mL methanol, and 5~10min of ultrasonic disperse heats up to being uniformly dispersed To 60~90 DEG C, 2~10mL quaternary ammonium salt functional reagents, 6~12h of back flow reaction is added dropwise.Room temperature is cooled to, Magneto separate, is used Milli-Q water washs for several times to acid-base value in neutrality, then with ethanol for several times, and 30~90 DEG C of 6~12h of vacuum drying, obtained carbon is received The immobilized quaternary ammonium salt magnetic functional material of mitron.
- 6. the immobilized quaternary ammonium salt magnetic functional material of CNT according to claim 5, it is characterised in that：The step (1) ammonia spirit is that content is at least one of 10% (V/V) and 25% (V/V) ammoniacal liquor in.
- 7. a kind of application of the immobilized quaternary ammonium salt magnetic functional material of CNT as described in any claim of Claims 1 to 4, its It is characterised by：20~100mg of the immobilized quaternary ammonium salt magnetic functional material of CNT is added to 100mL, and concentration is 5.0~500mg/ In L perchlorate solution, pH to 2~9 is adjusted, then 1~120min of constant temperature oscillation at 15~50 DEG C, that is, complete CNT Immobilized quaternary ammonium salt magnetic functional material goes the application of perchlorate in water removal.
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