CN102964496A - Preparation method of polystyrene-cobalt ferrite magnetic nanometer composite - Google Patents

Preparation method of polystyrene-cobalt ferrite magnetic nanometer composite Download PDF

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CN102964496A
CN102964496A CN2012105184036A CN201210518403A CN102964496A CN 102964496 A CN102964496 A CN 102964496A CN 2012105184036 A CN2012105184036 A CN 2012105184036A CN 201210518403 A CN201210518403 A CN 201210518403A CN 102964496 A CN102964496 A CN 102964496A
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polystyrene
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钟明
费鹏
付小瑞
邓超
张春娥
陈亚丽
苏碧桃
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Northwest Normal University
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Abstract

The invention provides a preparation method of a polystyrene-cobalt ferrite magnetic nanometer composite, and belongs to the technical field of composites. According to the preparation method, ferric chloride hexahydrate, cobalt chloride hexahydrate and styrene are used as raw materials, so that the polymerization of the styrene is realized while a cobalt ferrite (CoFe2O4) magnetic material is prepared, and the organic composition of the cobalt ferrite (CoFe2O4) and polystyrene (PS) is realized in one step through a hydrothermal method. According to the preparation method, the process is simple, the operation is convenient, the synthesis cost is low and the efficiency is high; and in the prepared PS-CoFe2O4 magnetic nanometer composite, by means of the chemical bonding effect between the organic and inorganic substances and the composition in the aspect of nanometer size, the comprehensive performance of the composite is effectively improved while the original characteristics of the PS-CoFe2O4 and the polystyrene are fully expressed, so that the application range of the composite is effectively expanded.

Description

The preparation method of a kind of polystyrene-vectolite magnetic nanometer composite material
Technical field
The invention belongs to technical field of composite materials, relate to a kind of preparation method of magnetic nanometer composite material, relate in particular to a kind of polystyrene-vectolite (PS-CoFe 2O 4) preparation method of magnetic nanometer composite material.
Background technology
Vectolite (the CoFe of spinel type ferrite 2O 4) magneticsubstance, owing to have unique physics, chemical property and magnetism characteristic, and its saturation magnetization is higher, magnetocrystalline anisotropy constant is larger, therefore better and the corrosion-resistant and wearing and tearing of chemical stability are having boundless application prospect aspect microwave absorbing, magnetic recording and the magnetic fluid.Yet, because Nanometer Cobalt Ferrite Oxide (CoFe 2O 4) between the magnetic-particle strong magnetic interaction cause the reunion between the nano particle, to a certain extent the magnetic performance of material caused detrimentally affect, and then has influence on Nanometer Cobalt Ferrite Oxide (CoFe 2O 4) application.
In order to be applicable to fields such as biological medicine, microelectronic product, information technology, katalysis, coating, magnetic fluid and electromagnetic interference shield, Magnetic polymer composite materials is subject to extensive concern as a kind of potential functional materials.Polystyrene (PS) is that molecular backbone chain is a kind of macromolecular material of non-conjugated structure, have good, the characteristics such as electrical insulating property is good, high-frequency dielectric, chemical resistance, water tolerance, easy-formation of the transparency, in composite manufacture, be widely used.Therefore, how to utilize vectolite (CoFe 2O 4) and the characteristics of polystyrene (PS), carry out the two compound and give its special performance, be the challenge that researcher faces.
At present, the method for preparing the PS-composite material of inorganic matter mainly comprises: the self-assembly method of situ aggregation method, microwave heating method, collosol and gel-pressure sintering, chemical coprecipitation, molecule etc.Yet have problems in the aforesaid method, as mostly need to carrying out the finishing of inorganic materials in the polymerization in position, and macromolecular grafted rate is low, material is easily reunited; Need the high-temperature calcination crystallization to process when utilizing for another example collosol and gel to prepare inorganic materials, and complicated process of preparation, productive rate are lower, and affect its large-scale production and application.
Summary of the invention
The objective of the invention is for problems of the prior art, the preparation method of a kind of polystyrene-vectolite magnetic nanometer composite material is provided.
The preparation method of polystyrene of the present invention-vectolite magnetic nanometer composite material is with Iron trichloride hexahydrate (FeCl 36H 2O), CoCL2 6H2O (CoCl 26H 2O), vinylbenzene (S) is raw material, with Potassium Persulphate (K 2S 2O 8) make catalyzer, under nitrogen environment, carry out hydro-thermal reaction; Centrifugal after reaction finishes, washing, drying obtain polystyrene-vectolite nano composite material.
Its chemical equation is expressed as follows:
Figure 130357DEST_PATH_IMAGE001
Figure 527840DEST_PATH_IMAGE002
Its concrete preparation technology is: with CoCl 26H 2O, FeCl 36H 2O is dissolved in the mixed solution of ethanol and intermediate water, regulates pH=8 ~ 11; Then change the tetrafluoroethylene reactor over to; And to reactor adding vinylbenzene and catalyzer K 2S 2O 8After logical nitrogen drains air, heat up and carry out hydro-thermal reaction; Centrifugal after reaction finishes, washing, drying can make PS-CoFe 2O 4Nano composite material.
Described Iron trichloride hexahydrate, CoCL2 6H2O, cinnamic mass ratio are: 1: 0.4: 0.4 ~ 1: 0.4: 2.1.
The consumption of described catalyzer Potassium Persulphate is 5% ~ 16 % of raw material total amount.
Described hydro-thermal reaction is at 140 ~ 180 ℃ of lower reaction 6 ~ 18h.
Described washing is that the solid after centrifugal is washed with dehydrated alcohol, redistilled water successively.
Described drying is to be 12 ~ 24h 80 ~ 100 ℃ of lower time of drying.
Below by the PS-CoFe of the means such as XRD, FT-IR, TG, SEM, VSM to the present invention's preparation 2O 4Magnetic nanometer composite material characterizes.
1, XRD analysis
Fig. 1 is the CoFe that the present invention prepares 2O 4(a) and PS-CoFe 2O 4(b) XRD figure.By the result of Fig. 1 as can be known, the CoFe in the matrix material 2O 4Be spinel structure, polymer PS does not affect its crystalline structure, but its crystal property is had certain influence; Do not observe the characteristic diffraction peak of PS among the figure, but in 2 θ=20 oNear Bao Feng has appearred, this amorphous structure with PS is relevant.CoFe 2O 4CoFe in the reduction of diffraction peak and broadening and the mixture 2O 4Content, little size and degree of crystallinity thereof etc. relevant.By the Scherrer formula ( D=K λ/βCos θ) can calculate CoFe 2O 4And PS-CoFe 2O 4Size be respectively: 34 nm, 21 nm.The above results explanation, PS has prevention CoFe 2O 4The effect that particle is grown up.
2, FT-IR analyzes
Fig. 2 is CoFe 2O 4, PS and PS-CoFe 2O 4FT-IR figure.The IR spectrogram of comparative sample is found: matrix material PS-CoFe 2O 4In corresponding to the variation of phenyl ring characteristic peak relative intensity on the PS side chain, the CoFe in the matrix material is described 2O 4Have strong interaction with PS, this effect may be the π-electron in the phenyl ring and CoFe on the PS side chain 2O 4In metal ion between coordination.
3, TG analyzes
Fig. 3 is PS and PS-CoFe 2O 4Thermogravimetric curve.By relatively learning PS and PS-CoFe 2O 4In the time of 282,314 ℃, begin obvious Weight lose respectively, this is that polystyrene begins to degrade in this temperature and causes; The two reaches the constant weight state at 408,418 ℃ respectively, shows that polystyrene degraded fully.The above results shows, matrix material PS-CoFe 2O 4In the thermostability of the purer PS of PS to get well, this result further specifies the CoFe in the matrix material 2O 4There is the chemical bonding effect with PS.
4, sem analysis
Fig. 4 is CoFe 2O 4And PS-CoFe 2O 4SEM figure.As seen from Figure 4, CoFe 2O 4And PS-CoFe 2O 4Formed by uniform amorphous nano particle, without phenomenon of phase separation.Illustrate that hydrothermal method can realize between inorganic phase and organic phase making with chemical bonds PS-CoFe 2O 4Nano composite material.
5, hysteresis curve analysis
Fig. 5 is under 180 ℃, 12 h conditions, CoFe 2O 4And PS-CoFe 2O 4The hysteresis curve of matrix material.When table 1 is 12 h, CoFe under 140 ~ 180 ℃ of conditions 2O 4, PS-CoFe 2O 4Magnetic parameter.When table 2 is 180 ℃, PS-CoFe under 6 ~ 18 h conditions 2O 4Magnetic parameter.Table 3 is under 180 ℃, 12 h conditions, the PS-CoFe of different content S 2O 4Magnetic parameter.Can find out PS-CoFe by Fig. 5 and table 1,2,3 2O 4The saturation magnetization of matrix material is weaker than inorganic materials CoFe 2O 4, and PS-CoFe 2O 4The coercive force of matrix material is then greater than inorganic materials CoFe 2O 4The magnetic of matrix material derives from the inorganic magnetic component, and the coercive force of material depends primarily on the surface anisotropy of scantling and material.Therefore, PS and CoFe 2O 4The compound CoFe that increased 2O 4The magneticanisotropy of material has strengthened the coercive force of matrix material.
Figure 256762DEST_PATH_IMAGE003
Figure 335576DEST_PATH_IMAGE004
Above-mentioned hysteresis curve and magnetic parameter show that the polystyrene of the present invention's preparation-vectolite nano composite material has good magnetic property, can be used as magnetic probe or absorbing material etc. and be applied in the aspects such as microelectronic product, biological medicine, coating.
In sum, the PS-CoFe of the present invention's preparation 2O 4In the magnetic nanometer composite material and since organic-inorganic between the chemical bonding effect and nanoscale on compound, make matrix material give full play to PS-CoFe 2O 4In the time of with the polystyrene primary characteristic, effectively improve the over-all properties of material, thereby effectively expanded its range of application.
In addition, the present invention is with Iron trichloride hexahydrate (FeCl 36H 2O), CoCL2 6H2O (CoCl 26H 2O), vinylbenzene (S) is raw material, carrying out vectolite (CoFe 2O 4) when magneticsubstance prepares, realized cinnamic polymerization, by hydrothermal method, a step has been realized vectolite (CoFe 2O 4) and the organic composite of polystyrene (PS), its technique is simple, and is easy to operate, and synthetic cost is low, efficient is high, is conducive to suitability for industrialized production.
Description of drawings
Fig. 1 is the CoFe that the present invention prepares 2O 4And PS-CoFe 2O 4XRD figure;
Fig. 2 is the CoFe that the present invention prepares 2O 4, PS and PS-CoFe 2O 4FT-IR figure;
Fig. 3 is PS and the PS-CoFe that the present invention prepares 2O 4Thermogravimetric curve;
Fig. 4 is the CoFe that the present invention prepares 2O 4And PS-CoFe 2O 4SEM figure;
Fig. 5 is the CoFe that the present invention prepares 2O 4And PS-CoFe 2O 4The hysteresis curve of matrix material under 180 ℃ of conditions.
Fig. 6 is the CoFe that the present invention prepares 2O 4And PS-CoFe 2O 4Matrix material under 180 ℃ of conditions, the hysteresis curve enlarged view of coercivity H between-600 ~ 600Oe.
Embodiment
Below by specific embodiment to PS-CoFe of the present invention 2O 4The preparation of nano composite material and the performance of nano composite material are described further.
Embodiment 1
Take by weighing 0.9518g CoCl 26H 2O, 2.1674g FeCl 36H 2O(Co 2+, Fe 3+Molar ratio be 1:2), be dissolved in the mixed solution of 30 mL dehydrated alcohols and 10 mL intermediate waters, magnetic agitation makes it dissolving, regulate its pH=10 with concentrated ammonia solution after, change the tetrafluoroethylene reactor over to; Add again 3 mL(2.73 g in the reactor) K of vinylbenzene and 0.6758g 2S 2O 8, after logical nitrogen drains air, in 180 ℃ of lower reaction 12 h; Reaction is centrifugal after finishing, and solid sample places in the vacuum drying oven after washing with dehydrated alcohol, redistilled water, and drying is 12 hours under 100 ℃, namely gets PS-CoFe 2O 4Nano magnetic composite materials.
PS-CoFe 2O 4Saturation magnetization 44.8 emu/g of nano magnetic composite materials, coercive force is 191.4 Oe.
Embodiment 2
Take by weighing 0.9518g CoCl 26H 2O, 2.1674g FeCl 36H 2O(Co 2+, Fe 3+Molar ratio be 1:2), be dissolved in the mixed solution of 30 mL dehydrated alcohols and 10 mL intermediate waters, magnetic agitation makes it dissolving, regulate its pH=10 with concentrated ammonia solution after, change the tetrafluoroethylene reactor over to; Add again 3 mL(2.73 g in the reactor) K of vinylbenzene and 0.6758g 2S 2O 8, after logical nitrogen drains air, in 160 ℃ of lower reaction 12 h; Reaction is centrifugal after finishing, and solid sample places in the vacuum drying oven after washing with dehydrated alcohol, redistilled water, and drying is 12 hours under 100 ℃, namely gets PS-CoFe 2O 4Nano magnetic composite materials.
PS-CoFe 2O 4The saturation magnetization 42.50emu/g of nano magnetic composite materials, coercive force are 58.52 Oe.
Embodiment 3
Take by weighing 0.9518g CoCl 26H 2O, 2.1674g FeCl 36H 2O(Co 2+, Fe 3+Molar ratio be 1:2), be dissolved in the mixed solution of 30 mL dehydrated alcohols and 10 mL intermediate waters, magnetic agitation makes it dissolving, regulate its pH=10 with concentrated ammonia solution after, change the tetrafluoroethylene reactor over to; Add again 3 mL(2.73 g in the reactor) K of vinylbenzene and 0.6758g 2S 2O 8, after logical nitrogen drains air, in 140 ℃ of lower reaction 12 h; Reaction is centrifugal after finishing, and solid sample places in the vacuum drying oven after washing with dehydrated alcohol, redistilled water, and drying is 12 hours under 100 ℃, namely gets PS-CoFe 2O 4Nano magnetic composite materials.
PS-CoFe 2O 4Saturation magnetization 17.52 emu/g of nano magnetic composite materials, coercive force is 42.01 Oe.
Embodiment 4
Take by weighing 0.9518g CoCl 26H 2O, 2.1674g FeCl 36H 2O(Co 2+, Fe 3+Molar ratio be 1:2), be dissolved in the mixed solution of 30 mL dehydrated alcohols and 10 mL intermediate waters, magnetic agitation makes it dissolving, regulate its pH=10 with concentrated ammonia solution after, change the tetrafluoroethylene reactor over to; Add again 3 mL(2.73 g in the reactor) K of vinylbenzene and 0.6758g 2S 2O 8, after logical nitrogen drains air, in 180 ℃ of lower reaction 18 h; Reaction is centrifugal after finishing, and solid sample places in the vacuum drying oven after washing with dehydrated alcohol, redistilled water, and drying is 12 hours under 100 ℃, namely gets PS-CoFe 2O 4Nano magnetic composite materials.
PS-CoFe 2O 4Saturation magnetization 39.69 emu/g of nano magnetic composite materials, coercive force is 235.86 Oe.
Embodiment 5
Take by weighing 0.9518g CoCl 26H 2O, 2.1674g FeCl 36H 2O(Co 2+, Fe 3+Molar ratio be 1:2), be dissolved in the mixed solution of 30 mL dehydrated alcohols and 10 mL intermediate waters, magnetic agitation makes it dissolving, regulate its pH=10 with concentrated ammonia solution after, change the tetrafluoroethylene reactor over to; Add again 3 mL(2.73 g in the reactor) K of vinylbenzene and 0.6758g 2S 2O 8, after logical nitrogen drains air, in 180 ℃ of lower reaction 15 h; Reaction is centrifugal after finishing, and solid sample places in the vacuum drying oven after washing with dehydrated alcohol, redistilled water, and drying is 12 hours under 100 ℃, namely gets PS-CoFe 2O 4Nano magnetic composite materials.
PS-CoFe 2O 4Saturation magnetization 46.56 emu/g of nano magnetic composite materials, coercive force is 223.49 Oe.
Embodiment 6
Take by weighing 0.9518g CoCl 26H 2O, 2.1674g FeCl 36H 2O(Co 2+, Fe 3+Molar ratio be 1:2), be dissolved in the mixed solution of 30 mL dehydrated alcohols and 10 mL intermediate waters, magnetic agitation makes it dissolving, regulate its pH=10 with concentrated ammonia solution after, change the tetrafluoroethylene reactor over to; Add again 3 mL(2.73 g in the reactor) K of vinylbenzene and 0.6758g 2S 2O 8, after logical nitrogen drains air, in 180 ℃ of lower reaction 9 h; Reaction is centrifugal after finishing, and solid sample places in the vacuum drying oven after washing with dehydrated alcohol, redistilled water, and drying is 12 hours under 100 ℃, namely gets PS-CoFe 2O 4Nano magnetic composite materials.
PS-CoFe 2O 4Saturation magnetization 38.95 emu/g of nano magnetic composite materials, coercive force is 203.26 Oe.
Embodiment 7
Take by weighing 0.9518g CoCl 26H 2O, 2.1674g FeCl 36H 2O(Co 2+, Fe 3+Molar ratio be 1:2), be dissolved in the mixed solution of 30 mL dehydrated alcohols and 10 mL intermediate waters, magnetic agitation makes it dissolving, regulate its pH=10 with concentrated ammonia solution after, change the tetrafluoroethylene reactor over to; Add again 3 mL(2.73 g in the reactor) K of vinylbenzene and 0.6758g 2S 2O 8, after logical nitrogen drains air, in 180 ℃ of lower reaction 6 h; Reaction is centrifugal after finishing, and solid sample places in the vacuum drying oven after washing with dehydrated alcohol, redistilled water, and drying is 12 hours under 100 ℃, namely gets PS-CoFe 2O 4Nano magnetic composite materials.
PS-CoFe 2O 4Saturation magnetization 39.60 emu/g of nano magnetic composite materials, coercive force is 118.01 Oe.
Embodiment 8
Take by weighing 0.9518g CoCl 26H 2O, 2.1674g FeCl 36H 2O(Co 2+, Fe 3+Molar ratio be 1:2), be dissolved in the mixed solution of 30 mL dehydrated alcohols and 10 mL intermediate waters, magnetic agitation makes it dissolving, regulate its pH=10 with concentrated ammonia solution after, change the tetrafluoroethylene reactor over to; Add again 5 mL(4.55 g in the reactor) K of vinylbenzene and 0.6758g 2S 2O 8, after logical nitrogen drains air, reactor is placed 180 ℃ of lower reaction 15 h.Reaction is centrifugal after finishing, and solid sample places in the vacuum drying oven after washing with dehydrated alcohol, redistilled water, and drying is 12 hours under 100 ℃, namely gets PS-CoFe 2O 4Nano magnetic composite materials.
PS-CoFe 2O 4Saturation magnetization 35.29 emu/g of nano magnetic material, coercive force is 247.64 Oe.
Embodiment 9
Take by weighing 0.9518g CoCl 26H 2O, 2.1674g FeCl 36H 2O(Co 2+, Fe 3+Molar ratio be 1:2), be dissolved in the mixed solution of 30 mL dehydrated alcohols and 10 mL intermediate waters, magnetic agitation makes it dissolving, regulate its pH=10 with concentrated ammonia solution after, change the tetrafluoroethylene reactor over to; Add again 1 mL(0.91 g in the reactor) K of vinylbenzene and 0.6758g 2S 2O 8, after logical nitrogen drains air, reactor is placed 180 ℃ of lower reaction 15 h.Reaction is centrifugal after finishing, and solid sample places in the vacuum drying oven after washing with dehydrated alcohol, redistilled water, and drying is 12 hours under 100 ℃, namely gets PS-CoFe 2O 4Nano magnetic composite materials.
PS-CoFe 2O 4Saturation magnetization 45.47 emu/g of nano magnetic material, coercive force is 153.18 Oe.
Embodiment 10
Take by weighing 0.9518g CoCl 26H 2O, 2.1674g FeCl 36H 2O(Co 2+, Fe 3+Molar ratio be 1:2), be dissolved in the mixed solution of 30 mL dehydrated alcohols and 10 mL intermediate waters, magnetic agitation makes it dissolving, regulate its pH=10 with concentrated ammonia solution after, change the tetrafluoroethylene reactor over to; Add again 3 mL(2.73 g in the reactor) K of vinylbenzene and 0.4224 g 2S 2O 8, after logical nitrogen drains air, reactor is placed 180 ℃ of lower reaction 15 h.Reaction is centrifugal after finishing, and solid sample places in the vacuum drying oven after washing with dehydrated alcohol, redistilled water, and drying is 12 hours under 100 ℃, namely gets PS-CoFe 2O 4Nano magnetic composite materials.
PS-CoFe 2O 4Saturation magnetization 42.76 emu/g of nano magnetic material, coercive force is 105.50 Oe.

Claims (7)

1. the preparation method of polystyrene-vectolite magnetic nanometer composite material is take Iron trichloride hexahydrate, CoCL2 6H2O, vinylbenzene as raw material, makes catalyzer with Potassium Persulphate, utilizes the hydrothermal method one-step synthesis under nitrogen environment; Centrifugal after reaction finishes, washing, drying obtain polystyrene-vectolite nano composite material.
2. the preparation method of polystyrene-vectolite magnetic nanometer composite material as claimed in claim 1 is characterized in that: with CoCl 26H 2O, FeCl 36H 2O is dissolved in the mixed solution of ethanol and intermediate water, regulates pH=8 ~ 11; Then change the tetrafluoroethylene reactor over to; And to reactor adding vinylbenzene and catalyzer K 2S 2O 8After logical nitrogen drains air, heat up and carry out hydro-thermal reaction; Centrifugal after reaction finishes, washing, drying can make PS-CoFe 2O 4Nano composite material.
3. the preparation method of polystyrene-vectolite magnetic nanometer composite material as claimed in claim 1 or 2, it is characterized in that: described Iron trichloride hexahydrate, CoCL2 6H2O, cinnamic mass ratio are: 1: 0.4: 0.4 ~ 1: 0.4: 2.1.
4. the preparation method of polystyrene-vectolite magnetic nanometer composite material as claimed in claim 1 or 2 is characterized in that: the consumption of described catalyst sulfuric acid potassium is 5 %～16 % of raw material total amount.
5. the preparation method of polystyrene-vectolite magnetic nanometer composite material as claimed in claim 1 or 2, it is characterized in that: described hydro-thermal reaction is at 140 ~ 180 ℃ of lower reaction 6 ~ 18 h.
6. the preparation method of polystyrene-vectolite magnetic nanometer composite material as claimed in claim 1 or 2, it is characterized in that: described washing is that the solid after centrifugal is washed with dehydrated alcohol, redistilled water successively.
7. the preparation method of polystyrene-vectolite magnetic nanometer composite material as claimed in claim 1 is characterized in that: described drying is to be 12 ~ 24 h 80 ~ 100 ℃ of lower time of drying.
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