CN106914228A - A kind of novel magnetic composite nano materials and its application - Google Patents
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Abstract
The invention discloses a kind of novel magnetic composite nano materials and its application, respectively with aniline, sodium thiosulfate, ferroso-ferric oxide, Ludox, polyethylene glycol etc. is disperseed by ultrasonic wave, magnetic agitation, and the modified method such as nitrogen deoxygenation prepares magnetic composite nano material.Novel magnetic composite nano materials have good effect in terms of the heavy metal in removing waste water.
Description
Technical field
The present invention relates to a kind of novel magnetic composite nano materials and its application, belong to water-treatment technology field.
Background technology
Heavy metal as the conventional water pollutant of a class, because it has toxicity higher, it is impossible to which the features such as degrading turns into water
Very harmful and one kind for receiving much concern in body pollution thing.With industrial expansion, the pollution problem of heavy metal becomes increasingly conspicuous.Mesh
Before untill, for the heavy metal pollution of water body, main processing method includes absorption method, chemical precipitation method, ion-exchange, film
Partition method, bio-flocculation process etc..But the heavy metal pollution effect to water body is not a kind of fine, New Magnetic Field Controlled that I invents at present
Property composite nano materials carry out processing good removal effect by various physics chemical actions to the heavy metal in water body.
The content of the invention
For the problem that above-mentioned prior art is present, the present invention provides a kind of novel magnetic composite nano materials to be used to remove
By the preparation method of the heavy metal in waste water.
To achieve these goals, the technical solution adopted by the present invention is：It is prepared by a kind of novel magnetic composite nano materials
Method.
Comprise the following steps：
Step 1, ferroso-ferric oxide is processed into 2h, ultrasonic disperse at least 20min, with centrifugation with the hydrochloric acid solution of 0.1mol/L
Machine is separated, deionized water is washed 5-10 times；
The good ferroso-ferric oxide of step 2, ultrasonic disperse is added to the mixing in ethanol, deionized water and concentrated ammonia liquor (28%)
(volume ratio 5 in solution:3:2) in), magnetic agitation 3h is then carried out；
Step 3, Ludox is added drop-wise in above-mentioned solution, is added dropwise with per minute 30 drop speed, the magnetic agitation when being added dropwise,
Continue magnetic agitation 5h after completion of dropwise addition；
Step 4 and then above-mentioned solution is carried out into microwave treatment 5h under nitrogen atmosphere, carrying out magnetic separation, use ethanol
Cyclic washing is washed with deionized water 5-10 times, tentatively prepared nanoscale magnetic core；
Step 5 and then preliminary obtained nanoscale magnetic core is added to polyethylene glycol again, in deionized water mixed solution
(volume ratio 10:1), nitrogen deoxygenation, while carrying out magnetic agitation 4h；
Step 6, by above-mentioned mixed solution by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then will
Reactor is put into microwave reactor and boosts to 300kpa with the speed of 30kap/min, and temperature is with the speed liter of 20 DEG C/min
To 300 DEG C, 12h is reacted under neon atmosphere；
Step 7 and then the filtering under vavuum pump, remove moisture under vacuum rotary evaporator, and 110 DEG C of vacuum drying chamber is done
It is dry, obtain multi-stage porous nanoscale magnetic core；
Step 8, aniline is added in glacial acetic acid solution, 100 DEG C of 3h of magnetic agitation oil bath heating；
Step 9 and then obtained multi-stage porous nanoscale magnetic core is added in above-mentioned solution, then carries out ultrasonic disperse,
Aniline monomer is set to be evenly distributed in multi-stage porous nanoscale magnetic core, while carrying out magnetic agitation 4h；
Step 10, sodium thiosulfate, and activating agent Sodium Polyacrylate are added in above-mentioned solution, in nitrogen deoxygenation
Under, magnetic agitation 4h；
Step 11, above-mentioned solution is reacted into 3h under microwave reactor 300k, 500kpa, then vavuum pump filtering, constant temperature
110 DEG C of drying box dries 12h；
Step 12, dried after be ground into powder, be placed in Muffle furnace in the carbon dioxide atmosphere of 40% argon gas+60%
Under, the time is 180 minutes, 680 DEG C of temperature, and 0.6MPa finally gives magnetic composite nano material, and sieve 30-40 mesh, 10ml silicon
Colloidal sol
Heavy metal of the above-mentioned nano material in waste water is removed has good effect.
Beneficial effect:A kind of novel magnetic composite nano materials of the present invention are used to remove preparing for the heavy metal received in waste water
Method, the magnetic composite nano material prepared has bigger specific surface area than general nano material, more organic than single, inorganic
The nanoscale magnetic core that nano material has more excellent physicochemical properties, preparation is inhaled than general nano material to metal ion
Attached energy is stronger, adds polyethylene glycol in preparation process, and the ultrasonically treated magnetic core for waiting preparation has hierarchical porous structure, can after adsorb each
The heavy metal of type, is that the complexing of the compound rear heavy metal ion of aniline is more excellent, moreover it is possible in absorbing and reducing water
Some heavy metal ion, and exchanged water in heavy metal ion reach more preferable heavy-metal ion removal effect.Pass through again
Calcined under the carbon dioxide atmosphere of 40% argon gas+60%, magnetic composite nano material physico-chemical property is further improved can make it
Varying environment is adapted to, also the impurity in duct removing can be more thoroughly calcined.Wherein produce ferroso-ferric oxide, aniline, matter
Amount (g) volume (ml) compares 20:1 sample.20g ferroso-ferric oxides, 1ml aniline, 10ml Ludox, 200ml ethanol, deionized water and
(volume ratio 5 in the mixed solution of concentrated ammonia liquor (28%):3:2)), 200ml polyethylene glycol, (volume in deionized water mixed solution
Than 10:1), 100ml glacial acetic acid, 5g sodium thiosulfate, 3g activating agent Sodium Polyacrylates, other configurations solution is prepared according to step.
And ferroso-ferric oxide is produced, aniline, quality (g) volume (ml) compares 19:1 sample.19g ferroso-ferric oxides, 1ml aniline, 10ml
Ludox, (volume ratio 5 in the mixed solution of 200ml ethanol, deionized water and concentrated ammonia liquor (28%):3:), 2) the poly- second two of 200ml
Alcohol, (volume ratio 10 in deionized water mixed solution:1), 100ml glacial acetic acid, 5g sodium thiosulfate, 3g activating agent polyacrylic acid
Sodium, other configurations solution is prepared according to step.Weight under both ratios in obtained magnetic composite nano material removal waste water
Metal effect is best.
Specific embodiment
Embodiment 1 produces ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 20:1 sample.20g ferroso-ferric oxides,
1ml aniline, 10ml Ludox, (volume ratio 5 in the mixed solution of 200ml ethanol, deionized water and concentrated ammonia liquor (28%):3:
2)), 200ml polyethylene glycol, (volume ratio 10 in deionized water mixed solution:1), 100ml glacial acetic acid, 5g sodium thiosulfate, 3g
Activating agent Sodium Polyacrylate, other configurations solution is prepared according to step.
Step 1,20g ferroso-ferric oxides are processed into 2h, ultrasonic disperse at least 20min with the hydrochloric acid solution of 0.1mol/L, used
Centrifuge is separated, deionized water is washed 5-10 times；
The good ferroso-ferric oxide of step 2, ultrasonic disperse is added to 200ml ethanol, deionized water and concentrated ammonia liquor (28%)
(volume ratio 5 in mixed solution:3:2) in), magnetic agitation 3h is then carried out；
Step 3,10ml Ludox is added drop-wise in above-mentioned solution, is added dropwise with per minute 30 drop speed, the magnetic force when being added dropwise
Stirring, continues magnetic agitation 5h after completion of dropwise addition；
Step 4 and then above-mentioned solution is carried out into microwave treatment 5h under nitrogen atmosphere, carrying out magnetic separation, use ethanol
Cyclic washing is washed with deionized water 5-10 times, tentatively prepared nanoscale magnetic core；
Step 5 and then preliminary obtained nanoscale magnetic core is added to 200ml polyethylene glycol again, deionized water mixing is molten
(volume ratio 10 in liquid:1), nitrogen deoxygenation, while carrying out magnetic agitation 4h；
Step 6, by above-mentioned mixed solution by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then will
Reactor is put into microwave reactor and boosts to 300kpa with the speed of 30kap/min, and temperature is with the speed liter of 20 DEG C/min
To 300 DEG C, 12h is reacted under neon atmosphere；
Step 7 and then the filtering under vavuum pump, remove moisture under vacuum rotary evaporator, and 110 DEG C of vacuum drying chamber is done
It is dry, obtain multi-stage porous nanoscale magnetic core；
Step 8,1ml aniline is added in 100ml glacial acetic acid solutions, 100 DEG C of 3h of magnetic agitation oil bath heating；
Step 9 and then obtained multi-stage porous nanoscale magnetic core is added in above-mentioned solution, then carries out ultrasonic disperse,
Aniline monomer is set to be evenly distributed in multi-stage porous nanoscale magnetic core, while carrying out magnetic agitation 4h；
Step 10,5g sodium thiosulfate, and 3g activating agent Sodium Polyacrylates are added in above-mentioned solution, are removed in nitrogen
Under oxygen, magnetic agitation 4h；
Step 11, above-mentioned solution is reacted into 3h under microwave reactor 300k, 500kpa, then vavuum pump filtering, constant temperature
110 DEG C of drying box dries 12h；
Step 12, dried after be ground into powder, be placed in Muffle furnace in the carbon dioxide atmosphere of 40% argon gas+60%
Under, the time is 180 minutes, 680 DEG C of temperature, and 0.6MPa finally gives magnetic composite nano material, and sieve 30-40 mesh.
Embodiment 2 produces ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 19:1 sample.19g ferroso-ferric oxides,
1ml aniline, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 3 produces ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 21:1 sample.21g ferroso-ferric oxides,
1ml aniline, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 4 produces ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 22:1 sample.22g ferroso-ferric oxides,
1ml aniline, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 5 produces ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 23:1 sample.23g ferroso-ferric oxides,
1ml aniline, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 6 produces ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 24:1 sample.24g ferroso-ferric oxides,
1ml aniline, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 7 produces ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 25:1 sample.25g ferroso-ferric oxides,
1ml aniline, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 8 produces ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 26:1 sample.26g ferroso-ferric oxides,
1ml aniline, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 9 produces ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 18:1 sample.18g ferroso-ferric oxides,
1ml aniline, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 10 produces ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 17:1 sample.17g ferroso-ferric oxides,
1ml aniline, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 11 produces ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 16:1 sample.16g ferroso-ferric oxides,
1ml aniline, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 12 produces ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 15:1 sample.15g ferroso-ferric oxides,
1ml aniline, other raw material dosages, operating procedure is as embodiment 1.
Embodiment 13 produces ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 14:1 sample.14g ferroso-ferric oxides,
1ml aniline, other raw material dosages, operating procedure is as embodiment 1.
Reference examples 1 produce ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 20:1 sample.20g ferroso-ferric oxides,
1ml aniline, does not carry out ultrasonic disperse treatment, other raw material dosages, and operating procedure is as embodiment 1.
Reference examples 2 produce ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 20:1 sample.20g ferroso-ferric oxides,
1ml aniline, does not carry out magnetic agitation, other raw material dosages, and operating procedure is as embodiment 1.
Reference examples 3 produce ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 20:1 sample.20g ferroso-ferric oxides,
1ml aniline, does not carry out microwave treatment, other raw material dosages, and operating procedure is as embodiment 1.
Reference examples 4 produce ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 20:1 sample.20g ferroso-ferric oxides,
1ml aniline, is not added to (volume in the mixed solution of 200ml ethanol, deionized water and concentrated ammonia liquor (28%) by ferroso-ferric oxide
Than 5:3:2), but in single deionized water, other raw material dosages, operating procedure is as embodiment 1.
Reference examples 5 produce ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 20:1 sample.20g ferroso-ferric oxides,
1ml aniline, when microwave reactor reacts not under neon atmosphere, but is carried out, other raw material dosages, operating procedure under air
As embodiment 1.
Reference examples 6 produce ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 20:1 sample.20g ferroso-ferric oxides,
1ml aniline, does not carry out nitrogen deoxygenation operation, other raw material dosages, and operating procedure is as embodiment 1.
Reference examples 7 produce ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 20:1 sample.20g ferroso-ferric oxides,
1ml aniline, calcines but single air calcination, other raw material dosages not under mixed gas, and operating procedure is with embodiment 1 one
Sample.
Reference examples 8 are produced and are added without the compound sample of aniline.Remove the behaviour being combined with aniline after synthesis multi-stage porous nanometer magnetic core
Make, other raw material dosages, operating procedure is as embodiment 1.
Test method
By 1L by heavy metal pollution water additions 0.05g magnetic composite nanos material I preparation, also one group blank
Group is added without the magnetic composite nano material of my preparation.
The content of beary metal added in magnetic composite nano material contamination water is detected after the 12h of table one
Test result indicate that：It can be found that magnetic composite nano material prepared by embodiment 1,2 is used to remove receives heavy metal
Heavy metal effect in pollutant effluents preferably, illustrates ferroso-ferric oxide, and aniline, quality (g) volume (ml) compares 20:1,19:1
Sample, the synergy between internal each several part is preferably to the heavy metal best results in removal contaminant water.It is obtained under other ratios
Magnetic composite nano material to be used for the heavy metal effect that removes in waste water general.Comparative example 1, comparative example 1,2, and 3,4,5,
6,7 can be found that.Do not carry out ultrasonic wave dispersion, magnetic agitation, microwave treatment, without ethanol, deionized water and concentrated ammonia liquor
(28%) (volume ratio 5 in mixed solution:3:2), but single deionized water, when microwave reactor reacts not in neon
Under atmosphere, but carried out under air, nitrogen deoxygenation, magnetic composite nano material obtained in calcination operation is used to go under different atmosphere
Except the heavy metal effect in waste water is bad.Comparative example 1, and comparative example 8 is it can be found that prepared magnetic Nano not compound with aniline
Heavy metal effect in material removal pollutant effluents is bad.
Claims (5)
1. a kind of novel magnetic composite nano materials, it is characterised in that with aniline, sodium thiosulfate, ferroso-ferric oxide, silicon is molten
Glue, polyethylene glycol etc. are disperseed by ultrasonic wave, magnetic agitation, and the modified method such as nitrogen deoxygenation prepares magnetic composite nano material
Material.
2. a kind of novel magnetic composite nano materials according to claim 1, it is characterised in that specific preparation method is such as
Under：
Step 1, ferroso-ferric oxide is processed into 2h, ultrasonic disperse at least 20min with the hydrochloric acid solution of 0.1mol/L, with centrifuge point
Washed 5-10 times from, deionized water；
The good ferroso-ferric oxide of step 2, ultrasonic disperse is added to the mixed solution in ethanol, deionized water and concentrated ammonia liquor (28%)
In (volume ratio 5:3:2) in), magnetic agitation 3h is then carried out；
Step 3, Ludox is added drop-wise in above-mentioned solution, is added dropwise with per minute 30 drop speed, the magnetic agitation when being added dropwise is added dropwise
Continue magnetic agitation 5h after end；
Step 4 and then above-mentioned solution is carried out into microwave treatment 5h under nitrogen atmosphere, carrying out magnetic separation, with ethanol and gone
Ion water washing cyclic washing 5-10 times, tentatively prepared nanoscale magnetic core；
Step 5 and then preliminary obtained nanoscale magnetic core is added to polyethylene glycol, (volume in deionized water mixed solution again
Than 10:1), nitrogen deoxygenation, while carrying out magnetic agitation 4h；
Step 6, by above-mentioned mixed solution by flow diverter pour into polytetrafluoroethylene (PTFE) be liner reactor in, then will reaction
Kettle is put into microwave reactor and boosts to 300kpa with the speed of 30kap/min, and temperature rises to 300 with the speed of 20 DEG C/min
DEG C, react 12h under neon atmosphere；
Step 7 and then filtered under vavuum pump, remove moisture under vacuum rotary evaporator, 110 DEG C of dryings of vacuum drying chamber,
Obtain multi-stage porous nanoscale magnetic core；
Step 8, aniline is added in glacial acetic acid solution, 100 DEG C of 3h of magnetic agitation oil bath heating；
Step 9 and then obtained multi-stage porous nanoscale magnetic core is added in above-mentioned solution, then carries out ultrasonic disperse, make benzene
Amine monomers are evenly distributed in multi-stage porous nanoscale magnetic core, while carrying out magnetic agitation 4h；
Step 10, sodium thiosulfate, and activating agent Sodium Polyacrylate are added in above-mentioned solution, under nitrogen deoxygenation, magnetic
Power stirs 4h；
Step 11, above-mentioned solution is reacted into 3h under microwave reactor 300k, 500kpa, then vavuum pump filtering, freeze-day with constant temperature
110 DEG C of case dries 12h；
Step 12, dried after be ground into powder, be placed in Muffle furnace calcine, the time be 180 minutes, 680 DEG C of temperature,
0.6MPa, finally gives magnetic composite nano material, and sieve 30-40 mesh.
3. a kind of novel magnetic composite nano materials according to claim 2, it is characterised in that the step 12, it is placed in
In calcining under the carbon dioxide atmosphere of 40% argon gas+60% in Muffle furnace.
4. application of a kind of novel magnetic composite nano materials as described in power 1-3 in terms of the heavy metal in removing waste water.
5. application according to claim 4, described heavy metal is Cr, pb or Mn.
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| CN113881644A (en) * | 2021-09-28 | 2022-01-04 | 江苏金迪克生物技术股份有限公司 | Method for removing host DNA in rabies vaccine |
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| CN113881644A (en) * | 2021-09-28 | 2022-01-04 | 江苏金迪克生物技术股份有限公司 | Method for removing host DNA in rabies vaccine |
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