CN103611536A - Pure-phase nickel ferrite nano material as well as preparation method thereof and preparation method of aromatic amine - Google Patents
Pure-phase nickel ferrite nano material as well as preparation method thereof and preparation method of aromatic amine Download PDFInfo
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Abstract
The invention discloses a pure-phase nickel ferrite nano material as well as a preparation method thereof and a preparation method of aromatic amine. The pure-phase nickel ferrite nano material provided by the invention is as follows: pure-phase nickel ferrite is an octahedral nano magnetic particle with particle diameter of 50 nm-120 nm. The preparation method of the pure-phase nickel ferrite nano material comprises the following steps of: uniformly mixing mixed salt liquor of a nickel salt and a ferric salt with mixed liquor of a surfactant, normal hexane and isopropanol; uniformly mixing an alkaline agent with the mixed liquor of the surfactant, normal hexane and isopropanol; and mixing the two liquor, heating and reacting, cooling, washing, and drying in vacuum to obtain a catalyst nickel ferrite. The invention further discloses a method of preparing aromatic amine by using the nickel ferrite as the catalyst, wherein the preparation method comprises the following step of: adding proper amount of the catalyst into liquor of an aromatic nitro-compound containing a ceriman amount of sodium borohydride to realize catalysis. The invention provides a pure-phase nickel ferrite catalyst which is economical, efficient and capable of being recycled as well as a method of preparing aromatic amine with low speed, quick speed and high efficiency.
Description
Technical field
The present invention relates to that nickel ferrite based magnetic loaded is received and preparation method thereof, arylamine preparation method's field, be specifically related to the preparation method of a kind of pure phase nickel ferrite based magnetic loaded nano material and preparation method thereof, a kind of arylamine.
Background technology
Arylamine is a kind of important organic intermediate and raw material, for the synthesis of agricultural chemicals, medicine, rubber chemicals, fuel and pigment, synthetic resin, textile auxiliary, surfactant, photosensitive material etc.Arylamine can be obtained by corresponding nitro-aromatic compound reduction.Method of reducing has a lot, and wherein borohydride reduction nitro-aromatic compound is because reaction condition is gentle, reaction speed is fast, productive rate is high and process simply receives much concern.When using boron hydride to reduce, need to add catalyst, the heterogeneous catalysis for arylamine mainly concentrates on noble metal at present, Au simple substance for example, Ag simple substance, Pt/C compound, Ag/SiO
2compound, Pt-Ni is catalyst etc.; Also the nitro-aromatic compound that can reduce under excessive sodium borohydride condition is arylamine.Although the excellent performance of these catalyst, but the fancy price of noble metal own, catalyst are difficult to the use that the shortcomings such as recycling have seriously limited such catalyst, and boron hydride is expensive, use excessive boron hydride to improve especially production cost, be difficult to meet the course of industrialization of day by day pursuing high benefit.
The ferrite MFe with spinel structure
2o
4, wherein M=Fe, Co, Ni, Cu, be one of most important magnetic material, in ferrospinel, nickel ferrite based magnetic loaded is a kind of magnetic material of the inverse spinel structure being widely known by the people, and has ferrimagnetism and comes from four sides position Fe
3+ion and octahedral position Ni
2+the magnetic moment of the antiparallel spin between ion.Nickel ferrite based magnetic loaded nanocrystal is because of its unique physical and chemical performance, comprise moderate saturation magnetization, high Curie temperature, excellent chemically stable and high mechanical hardness and get most of the attention, being widely used in the fields such as magnetic resonance imaging, energy transfer, storage, catalyst, sensing technology and spintronics.
Therefore, use transition-metals and their oxides as catalyst, it is an effective approach that direct catalytic reduction nitro-aromatic compound is prepared arylamine.
Summary of the invention:
The technical problem that the present invention will solve is to provide a kind of pure phase nickel ferrite based magnetic loaded nano material.
Another technical problem that the present invention will solve is to provide a kind of preparation method of pure phase nickel ferrite based magnetic loaded nano material.
The technical problem that the present invention also will solve is to provide a kind of preparation method of arylamine.
For solving the problems of the technologies described above, the invention provides a kind of pure phase nickel ferrite based magnetic loaded nano material: pure phase nickel ferrite based magnetic loaded is octahedra nano magnetic particle, particle diameter is 50-120nm.
The preparation method who the invention provides a kind of pure phase nickel ferrite based magnetic loaded nano material, comprises the following steps:
A, surfactant and n-hexane and isopropyl alcohol are uniformly mixed, obtain solution A; Surfactant and n-hexane and isopropyl alcohol are uniformly mixed, obtain solution B;
B, get the mixing salt solution that nickel salts and metal molysite are made into, dropwise join in solution A, stir 20-40 minute, obtain suspension A, alkaline agent is dropwise joined in described solution B, stir 20-40 minute, obtain suspension B;
C, suspension B is dropwise added in suspending liquid A, stirs 2-4h, obtain emulsion;
D, emulsion is poured in the stainless steel still that liner is polytetrafluoroethylene (PTFE), heating, isothermal reaction, then naturally cools to room temperature, obtains rufous product;
E, by steps d products therefrom with cleaning 3-6 time with ethanol again after washed with de-ionized water 3-6 time, product vacuum drying is dried, obtain catalyst nickel ferrite based magnetic loaded.
Described in step a, surfactant is softex kw.
Nickel mol ratio in the A of suspension described in step b in surfactant and nickel salts is 5:1-40:1, nickel mol ratio in suspension A in n-hexane and nickel salts is 200:1-1500:1, and the nickel mol ratio in suspension A in isopropyl alcohol and nickel salts is 20:1-1000:1; In described suspension B, in surfactant and suspension A, the nickel mol ratio in nickel salts is 9:1-50:1, in described suspension B, in n-hexane and suspension A, the mol ratio of the nickel in nickel salts is 240:1-1900:1, and in described suspension B, in isopropyl alcohol and suspension A, the nickel mol ratio in nickel salts is 150:1-1200:1.
The ratio that step b gets the amount of substance of nickel salts and metal molysite in mixing salt solution is the nickel in nickel salts: the iron=1:2 of metal molysite.
Described in step b nickel salts be Nickel dichloride hexahydrate or six hydration nickel sulfate any one, metal molysite be Fe(NO3)39H2O or six hydration ferric sesquichlorides any one.
Described in step b, alkaline agent is: NaOH or potassium hydroxide any one, concentration is 0.25-1.50mol/L, and in suspension B, in alkaline agent and suspension A, the ratio of the nickel amount of substance in nickel salts is alkaline agent in suspension B: the nickel=3:1-150:1 in suspension A in nickel salts.
Isothermal reaction described in steps d is 150-190 ℃ of reaction 12-18h.
Described in step e, vacuum drying is dry 6-24h at 25-60 ℃.
The invention also discloses the preparation method of arylamine, is catalyst by the prepared pure phase nickel ferrite based magnetic loaded of the present invention, and catalytic reduction nitro-aromatic compound obtains arylamine.
The method that nickel ferrite based magnetic loaded is prepared arylamine as catalyst at catalytic reduction nitro-aromatic compound is:
Appropriate sodium borohydride solution is mixed with the solution of the nitro-aromatic compound that contains appropriate nickel ferrite based magnetic loaded, realize catalysis.Because this catalytic process is pseudo first order reaction, the mol ratio of sodium borohydride and nitro-aromatic compound is sodium borohydride: nitro-aromatic compound=100-2000:1.
Concrete steps are as follows:
(1) prepare the sodium borohydride solution of appropriate concentration, sodium borohydride and nitro-aromatic compound mol ratio are sodium borohydride: nitro-aromatic compound=100-2000:1.
(2), according to mol ratio nickel ferrite based magnetic loaded: p-nitrophenol=5-20:1, take catalyst nickel ferrite based magnetic loaded prepared by appropriate the present invention and join in p-nitrophenol, and be made into mixed solution.
(3) by step (1) and the ultrasonic dispersion 2-5min of step (2) products therefrom difference, after both are mixed, static, every sampling in 10 minutes once, with Shanghai unit, analyse UV-6100s spectrophotometer testing catalytic effect, transparent by xanthochromia to solution colour, finish test.
(4) with magnet, reclaim catalyst, after ultrasonic cleaning,, reuse.
The nucleation process of nickel ferrite based magnetic loaded can be thought two-step reaction:
(1) molysite and nickel salt form iron hydroxide and nickel hydroxide under alkali condition
(2) iron hydroxide and nickel hydroxide form the NiFe of intermediate state
2(OH)
8, finally dehydration obtains nickel ferrite based magnetic loaded.
In the present invention, alkaline agent provides alkaline environment and has promoted the carrying out reacting.Surfactant to organic solvent played disperse and and the effect of increase-volume, reduced reaction institute energy requirement, be more conducive to nucleation and the generation of pure phase nickel ferrite based magnetic loaded.
The present invention is by regulating the pattern of product by different alkaline agents and adjusting reaction temperature.Potassium hydroxide can obtain the nickel ferrite based magnetic loaded of polyhedral structure as alkaline agent and with the nano particle of more not yet nucleation; Ammoniacal liquor can only obtain nano particle as alkaline agent, cannot obtain having the nanocrystal of certain pattern.Too low temperature is unfavorable for the growth of crystal, and too high temperature has certain destruction to the pattern of product.The growth of crystal is also relevant with the time of reaction, and the time is too short, and the growth of crystal is incomplete, between overlong time crystal, can produce and merge.The consumption of alkaline agent also can affect the pattern of product to a certain extent.
The pure phase nanometer nickel ferrite based magnetic loaded catalyst energy catalytic reduction p-nitrophenol that the present invention is prepared, and can realize after repeatedly recycling and still keep higher catalytic activity, and its good magnetic property makes it be easy to separate from reacted solution, can repeatedly reclaim, recycle, aspect chemical industry, have a good application prospect.The method of preparing arylamine provided by the invention, cost is low, and speed is fast, and efficiency is high, is applicable to industrial production.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction pattern of embodiment 2 gained catalyst.
Fig. 2 is the energy-dispersive X-ray analysis spectrogram of embodiment 2 gained catalyst.
Fig. 3 (a) is the electron scanning micrograph of embodiment 1 gained catalyst.
Fig. 3 (b) is the electron scanning micrograph of embodiment 2 gained catalyst.
Fig. 3 (c) is the electron scanning micrograph of embodiment 3 gained catalyst.
Fig. 3 (d) is the electron scanning micrograph of embodiment 4 gained catalyst.
Fig. 3 (e) is the electron scanning micrograph of embodiment 5 gained catalyst.
Fig. 4 is the room temperature hysteresis curve of embodiment 2 gained catalyst.
Fig. 5 is that the UV, visible light of embodiment 2 gained catalyst p-nitrophenols absorbs spectrogram.
Fig. 6 is that the different amounts 6,9 of catalyst of embodiment 2 preparations is, the UV, visible light of 12mg catalysis p-nitrophenol absorbs spectrogram.
Fig. 7 (a) is that 10 cycling and reutilization testing time-residual concentrations of different amounts catalysis of catalyst of embodiment 2 preparation are than figure.
Fig. 7 (b) is 10 cycling and reutilization test loop number of times-catalytic rate figure of different amounts catalysis of the catalyst of embodiment 2 preparation.
Fig. 8 is the catalyst p-nitrophenol ln (C of embodiment 2 preparations
t/ C
0) and the graph of a relation of reaction time t.
Fig. 9 is that the UV, visible light of catalyst 2-nitrophenol, paranitroanilinum and 2, the 4-dinitroaniline of embodiment 2 preparations absorbs spectrogram.
Figure 10 is the ln (C of catalyst 2-nitrophenol, paranitroanilinum and 2, the 4-dinitroaniline of embodiment 2 preparations
t/ C
0) and the graph of a relation of reaction time t.
The specific embodiment
Fig. 3 (a) is depicted as the pure phase nickel ferrite based magnetic loaded electron scanning micrograph of embodiment 1 preparation, is octahedra nano magnetic particle, and particle diameter is 70nm.
The preparation method of pure phase nickel ferrite based magnetic loaded nano material, comprises the following steps:
A, the isopropyl alcohol of the n-hexane of 1mmol softex kw and 5mL and 1.7mL is uniformly mixed, obtains solution A; The isopropyl alcohol of the n-hexane of the softex kw of 1.5mmol and 5mL and 2.5mL is uniformly mixed, obtains solution B;
B, get the mixing salt solution that 0.7mL Nickel dichloride hexahydrate and Fe(NO3)39H2O are made into, dropwise join in described solution A, stir 20 minutes, obtain suspension A, institute gets and in 0.7mL mixing salt solution, contains Nickel dichloride hexahydrate 0.125mmol and Fe(NO3)39H2O 0.25mmol; The potassium hydroxide solution of 6mL0.5mol/L is dropwise joined in described solution B, stir 20 minutes, obtain suspension B;
C, suspension B is dropwise added in suspending liquid A, then stirs 2h, obtain emulsion;
D, emulsion is poured in the stainless steel still that liner is polytetrafluoroethylene (PTFE), be heated to 150 ℃, isothermal reaction 18h, naturally cools to room temperature, obtains rufous product;
E, by deionized water washing for products therefrom 3 times, then with after ethanol washing 3 times, by product vacuum drying 24h at 25 ℃, obtain catalyst nickel ferrite based magnetic loaded.
Fig. 3 (b) is depicted as the pure phase nickel ferrite based magnetic loaded electron scanning micrograph of embodiment 2 preparations, is octahedra nano magnetic particle, and particle diameter is 80nm.
The preparation method of pure phase nickel ferrite based magnetic loaded nano material, comprises the following steps:
A, the n-hexane of 5mmol softex kw 25mL and the isopropyl alcohol of 9.2mL are uniformly mixed, obtain solution A; The isopropyl alcohol of the n-hexane of 6mmol softex kw and 30mL and 11mL is uniformly mixed, obtains solution B;
B, get 2mL Nickel dichloride hexahydrate and Fe(NO3)39H2O mixing salt solution, dropwise join in described solution A, stir 30 minutes, obtain suspension A, the 2mL mixing salt solution of getting contains Nickel dichloride hexahydrate 0.376mmol and Fe(NO3)39H2O 0.752mmol; The sodium hydroxide solution of 10mL1mol/L is dropwise joined in described solution B, stir 30 minutes, obtain suspension B;
C, suspension B is dropwise added in suspending liquid A, then stirs 3h, obtain emulsion;
D, emulsion is poured in the stainless steel still that 50mL liner is polytetrafluoroethylene (PTFE), be heated to 170 ℃, isothermal reaction 15h, naturally cools to room temperature, obtains rufous product;
E, by products therefrom with after deionized water washing 4 times, then with ethanol washing 4 times, by product vacuum drying 12h at 60 ℃, obtain catalyst nickel ferrite based magnetic loaded.
Fig. 3 (c) is depicted as the pure phase nickel ferrite based magnetic loaded electron scanning micrograph of embodiment 3 preparations, is octahedra nano magnetic particle, and particle diameter is 100nm.
The preparation method of pure phase nickel ferrite based magnetic loaded nano material, comprises the following steps:
A, the n-hexane of 1.5mmol softex kw 17mL and the isopropyl alcohol of 6.1mL are uniformly mixed, obtain solution A; The isopropyl alcohol of the n-hexane of 8mmol softex kw and 20mL and 5.5mL is uniformly mixed, obtains solution B;
B, get the mixing salt solution that 1.2mL six hydration nickel sulfate and six hydration ferric sesquichlorides are made into, dropwise join in described solution A, stir 40 minutes, obtain suspension A, institute gets and in mixing salt solution, contains six hydration nickel sulfate 0.225mmol and ferric chloride hexahydrate 0.45mol; The sodium hydroxide solution of 12mL0.25mol/L is dropwise joined in described solution B, stir 40 minutes, obtain suspension B;
C, suspension B is dropwise added in suspending liquid A, then stirs 4h, obtain emulsion;
D, to pour emulsion into 50mL liner be that polytetrafluoroethylene (PTFE) obtains in stainless steel still, is heated to 190 ℃, and isothermal reaction 12h, naturally cools to room temperature, obtains rufous product;
E, by products therefrom with after deionized water washing 6 times, then with ethanol washing 6 times, by product vacuum drying 6h at 60 ℃, obtain catalyst nickel ferrite based magnetic loaded.
Fig. 3 (d) is depicted as the pure phase nickel ferrite based magnetic loaded electron scanning micrograph of embodiment 4 preparations, is octahedra nano magnetic particle, and particle diameter is 120nm.
The preparation method of pure phase nickel ferrite based magnetic loaded nano material, comprises the following steps:
A, the n-hexane of 7.5mmol softex kw 35mL and the isopropyl alcohol of 16mL are uniformly mixed, obtain solution A; The isopropyl alcohol of the n-hexane of 10mmol softex kw and 45mL and 20mL is uniformly mixed, obtains solution B;
B, get the mixing salt solution that 1.2mL Nickel dichloride hexahydrate and six hydration ferric sesquichlorides are made into, dropwise join in described solution A, stir 30 minutes, obtain suspension A, institute gets and in mixing salt solution, contains Nickel dichloride hexahydrate 0.225mmol and ferric chloride hexahydrate 0.45mol; The sodium hydroxide solution of 20mL1.5mol/L is dropwise joined in described solution B, stir 30 minutes, obtain suspension B;
C, suspension B is dropwise added in suspending liquid A, then stirs 3h, obtain emulsion;
D, to pour emulsion into 50mL liner be that polytetrafluoroethylene (PTFE) obtains in stainless steel still.Be heated to 170 ℃, isothermal reaction 15h, naturally cools to room temperature, obtains rufous product;
E, by products therefrom with after deionized water washing 4 times, then with ethanol washing 4 times, by product vacuum drying 12h at 60 ℃, obtain catalyst nickel ferrite based magnetic loaded.
Fig. 3 (e) is depicted as the pure phase nickel ferrite based magnetic loaded electron scanning micrograph of embodiment 5 preparations, is octahedra nano magnetic particle, and particle diameter is 110nm.
The preparation method of pure phase nickel ferrite based magnetic loaded nano material, comprises the following steps:
A, the n-hexane of 4.5mmol softex kw 10mL and the isopropyl alcohol of 3.1mL are uniformly mixed, obtain solution A; The isopropyl alcohol of the n-hexane of 6mmol softex kw and 20mL and 5.5mL is uniformly mixed, obtains solution B;
B, get the mixing salt solution that 1.2mL six hydration nickel sulfate and Fe(NO3)39H2O are made into, dropwise join in described solution A, stir 30 minutes, obtain suspension A, institute gets and in mixing salt solution, contains six hydration nickel sulfate 0.225mmol and Fe(NO3)39H2O 0.45mmol; The sodium hydroxide solution of 8mL1mol/L is dropwise joined in described solution B, stir 30 minutes, obtain suspension B;
C, suspension B is dropwise added in suspending liquid A, then stirs 3h, obtain latex A;
D, to pour latex A into 50mL liner be that polytetrafluoroethylene (PTFE) obtains in stainless steel still.Be heated to 170 ℃, isothermal reaction 15h, naturally cools to room temperature, obtains rufous product;
E, products therefrom is cleaned respectively after 4 times with deionized water and ethanol, by product vacuum drying 12h at 60 ℃, obtain nickel ferrite based magnetic loaded.
Nickel ferrite based magnetic loaded prepared by the present invention is prepared the method for arylamine as catalyst reduction nitro-aromatic compound, comprise the steps:
(1) prepare the sodium borohydride solution that concentration is 0.12mol/L, measure 11.2ml standby;
(2) take catalyst nickel ferrite based magnetic loaded prepared by the present invention of 3mg and join in the p-nitrophenyl phenol solution of 15mL0.18mmol/L, be i.e. mol ratio nickel ferrite based magnetic loaded: p-nitrophenol=5:1;
(3) by step (1) and the ultrasonic dispersion 2min of step (2) products therefrom difference, after both are mixed, static, every sampling in 10 minutes once, with Shanghai unit, analyse UV-6100s spectrophotometer testing catalytic effect, within 140 minutes, solution colour is transparent by xanthochromia, finishes test.
(4) with magnet, reclaim catalyst, after ultrasonic cleaning,, reuse.
Nickel ferrite based magnetic loaded prepared by the present invention is prepared the method for arylamine as catalyst reduction nitro-aromatic compound, comprise the steps:
(1) prepare the sodium borohydride solution that concentration is 0.236mol/L, measure 11.2ml standby;
(2) take catalyst nickel ferrite based magnetic loaded prepared by the present invention of 9mg and join in the 2-nitrophenol solution of 15mL0.18mmol/L, be i.e. mol ratio nickel ferrite based magnetic loaded: 2-nitrophenol=15:1;
(3) by step (1) and the ultrasonic dispersion 2min of step (2) products therefrom difference, after both are mixed, static, every sampling in 10 minutes once, with Shanghai unit, analyse UV-6100s spectrophotometer testing catalytic effect, within 80 minutes, solution colour is transparent by xanthochromia, finishes test.
(4) with magnet, reclaim catalyst, after ultrasonic cleaning,, reuse.
Nickel ferrite based magnetic loaded prepared by the present invention is prepared the method for arylamine as catalyst reduction nitro-aromatic compound, comprise the steps:
(1) prepare the sodium borohydride solution that concentration is 0.18mol/L, measure 11.2ml standby;
(2) take catalyst nickel ferrite based magnetic loaded prepared by the present invention of 12mg and join in the 2-nitrophenol solution of 15mL0.18mmol/L, be i.e. mol ratio nickel ferrite based magnetic loaded: 2-nitrophenol=20:1;
(3) by step (1) and the ultrasonic dispersion 2min of step (2) products therefrom difference, after both are mixed, static, every sampling in 10 minutes once, with Shanghai unit, analyse UV-6100s spectrophotometer testing catalytic effect, within 80 minutes, solution colour is transparent by xanthochromia, finishes test.
(4) with magnet, reclaim catalyst, after ultrasonic cleaning,, reuse.
Nickel ferrite based magnetic loaded prepared by the present invention is prepared the method for arylamine as catalyst reduction nitro-aromatic compound, comprise the steps:
(1) prepare the sodium borohydride solution that concentration is 0.236mol/L, measure 11.2ml standby;
(2) take catalyst nickel ferrite based magnetic loaded prepared by the present invention of 9mg and join in the 2-nitrophenol solution of 15mL0.24mmol/L, be i.e. mol ratio nickel ferrite based magnetic loaded: 2-nitrophenol=15:1;
(3) by step (1) and the ultrasonic dispersion 2min of step (2) products therefrom difference, after both are mixed, static, every sampling in 10 minutes once, with Shanghai unit, analyse UV-6100s spectrophotometer testing catalytic effect, within 80 minutes, solution colour is transparent by xanthochromia, finishes test.
(4) with magnet, reclaim catalyst, after ultrasonic cleaning,, reuse.
Nickel ferrite based magnetic loaded prepared by the present invention is prepared the method for arylamine as catalyst reduction nitro-aromatic compound, comprise the steps:
(1) prepare the sodium borohydride solution that concentration is 0.18mol/L, measure 11.2ml standby;
(2) take catalyst nickel ferrite based magnetic loaded prepared by the present invention of 9mg and join in the p-nitrophenyl amine aqueous solution of 15mL0.18mmol/L, be i.e. mol ratio nickel ferrite based magnetic loaded: paranitroanilinum=15:1;
(3) by step (1) and the ultrasonic dispersion 3min of step (2) products therefrom difference, after both are mixed, static, every sampling in 10 minutes once, with Shanghai unit, analyse UV-6100s spectrophotometer testing catalytic effect, within 70 minutes, solution colour is transparent by xanthochromia, finishes test.
(4) with magnet, reclaim catalyst, after ultrasonic cleaning,, reuse.
Embodiment 11
Nickel ferrite based magnetic loaded prepared by the present invention is prepared the method for arylamine as catalyst reduction nitro-aromatic compound, comprise the steps:
(1) prepare the sodium borohydride solution that concentration is 0.18mol/L, measure 11.2ml standby;
(2) take catalyst nickel ferrite based magnetic loaded prepared by the present invention of 9mg and join in the 2,4-DNP solution of 15mL0.18mmol/L, be i.e. mol ratio nickel ferrite based magnetic loaded: 2,4-DNP=15:1;
(3) by step (1) and the ultrasonic dispersion 3min of step (2) products therefrom difference, after both are mixed, static, every sampling in 10 minutes once, with Shanghai unit, analyse UV-6100s spectrophotometer testing catalytic effect, within 100 minutes, solution colour is transparent by xanthochromia, finishes test.
(4) with magnet, reclaim catalyst, after ultrasonic cleaning,, reuse.
The above is only the preferred embodiment of the present invention; be noted that for a person skilled in the art, under the premise without departing from the principles of the invention, can also make some improvements and modifications; these improvements and modifications, all should be considered as protection scope of the present invention.
Claims (10)
1. a pure phase nickel ferrite based magnetic loaded nano material, is characterized in that pure phase nickel ferrite based magnetic loaded is octahedra nano magnetic particle, and particle diameter is 50-120nm.
2. the preparation method of pure phase nickel ferrite based magnetic loaded nano material claimed in claim 1, is characterized in that comprising the following steps:
A, surfactant and n-hexane and isopropyl alcohol are uniformly mixed, obtain solution A; Surfactant and n-hexane and isopropyl alcohol are uniformly mixed, obtain solution B;
B, get the mixing salt solution that nickel salts and metal molysite are made into, dropwise join in solution A, stir 20-40 minute, obtain suspension A, alkaline agent is dropwise joined in described solution B, stir 20-40 minute, obtain suspension B;
C, suspension B is dropwise added in suspending liquid A, stirs 2-4h, obtain emulsion;
D, emulsion is poured in the stainless steel still that liner is polytetrafluoroethylene (PTFE), heating, isothermal reaction, then naturally cools to room temperature, obtains rufous product;
E, by steps d products therefrom with cleaning 3-6 time with ethanol again after washed with de-ionized water 3-6 time, product vacuum drying is dried, obtain catalyst nickel ferrite based magnetic loaded.
3. the preparation method of pure phase nickel ferrite based magnetic loaded nano material according to claim 2, is characterized in that: described in step a, surfactant is softex kw.
4. the preparation method of pure phase nickel ferrite based magnetic loaded nano material according to claim 2, it is characterized in that: the nickel mol ratio in described suspension A in surfactant and nickel salts is 5:1-40:1, nickel mol ratio in suspension A in n-hexane and nickel salts is 200:1-1500:1, and the nickel mol ratio in suspension A in isopropyl alcohol and nickel salts is 20:1-1000:1; In described suspension B, in surfactant and suspension A, the nickel mol ratio in nickel salts is 9:1-50:1, in described suspension B, in n-hexane and suspension A, the mol ratio of the nickel in nickel salts is 240:1-1900:1, in described suspension B, in isopropyl alcohol and suspension A, the nickel mol ratio in nickel salts is 150:1-1200:1, get the amount of substance of nickel salts and metal molysite in mixing salt solution ratio be the nickel in nickel salts: the iron=1:2 of metal molysite.
5. the preparation method of pure phase nickel ferrite based magnetic loaded nano material according to claim 2, it is characterized in that: described in step b nickel salts be Nickel dichloride hexahydrate or six hydration nickel sulfate any one, metal molysite be Fe(NO3)39H2O or six hydration ferric sesquichlorides any one.
6. the preparation method of pure phase nickel ferrite based magnetic loaded nano material according to claim 2, it is characterized in that: described in step b, alkaline agent is: NaOH or potassium hydroxide any one, concentration is 0.25-1.50mol/L, and in suspension B, in alkaline agent and suspension A, the ratio of the nickel amount of substance in nickel salts is alkaline agent in suspension B: the nickel=3:1-150:1 in suspension A in nickel salts.
7. the preparation method of pure phase nickel ferrite based magnetic loaded nano material according to claim 2, is characterized in that: isothermal reaction described in steps d is 150-190 ℃ of reaction 12-18h.
8. the preparation method of pure phase nickel ferrite based magnetic loaded nano material according to claim 2, is characterized in that: described in step e, vacuum drying is dry 6-24h at 25-60 ℃.
9. a preparation method for arylamine, is characterized in that: utilize pure phase nickel ferrite based magnetic loaded nano material as catalyst.
10. the preparation method of arylamine according to claim 9, is characterized in that comprising the following steps:
(1) prepare the sodium borohydride solution of appropriate concentration, sodium borohydride and nitro-aromatic compound mol ratio are sodium borohydride: nitro-aromatic compound=100-2000:1.
(2), according to mol ratio nickel ferrite based magnetic loaded: p-nitrophenol=5-20:1, take catalyst nickel ferrite based magnetic loaded prepared by appropriate the present invention and join in p-nitrophenol, and be made into mixed solution.
(3) by step (1) and the ultrasonic dispersion 2-5min of step (2) products therefrom difference, after both are mixed, static, every sampling in 10 minutes once, with Shanghai unit, analyse UV-6100s spectrophotometer testing catalytic effect, transparent by xanthochromia to solution colour, finish test.
(4) with magnet, reclaim catalyst, after ultrasonic cleaning,, reuse.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106345438A (en) * | 2015-07-15 | 2017-01-25 | 江南石墨烯研究院 | Preparation method for magnetic water body adsorbing agent with controllable structure and morphology |
| CN110102304A (en) * | 2019-04-03 | 2019-08-09 | 江苏载驰科技股份有限公司 | A kind of preparation method and application of ferrous acid Raney nickel |
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| CN106345438A (en) * | 2015-07-15 | 2017-01-25 | 江南石墨烯研究院 | Preparation method for magnetic water body adsorbing agent with controllable structure and morphology |
| CN110102304A (en) * | 2019-04-03 | 2019-08-09 | 江苏载驰科技股份有限公司 | A kind of preparation method and application of ferrous acid Raney nickel |
| CN117820129A (en) * | 2023-12-29 | 2024-04-05 | 南京先进生物材料与过程装备研究院有限公司 | Method for preparing corresponding aromatic amine by selective hydrogenation of photocatalytic aromatic nitro compound |
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