CN106745294A - Device and application prepared by a kind of parallel high temperature pyrolysis of magnetic nanoparticle - Google Patents
Device and application prepared by a kind of parallel high temperature pyrolysis of magnetic nanoparticle Download PDFInfo
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- CN106745294A CN106745294A CN201610977008.2A CN201610977008A CN106745294A CN 106745294 A CN106745294 A CN 106745294A CN 201610977008 A CN201610977008 A CN 201610977008A CN 106745294 A CN106745294 A CN 106745294A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/009—Compounds containing, besides iron, two or more other elements, with the exception of oxygen or hydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
- C01G49/0063—Mixed oxides or hydroxides containing zinc
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The device prepared the invention discloses a kind of parallel high temperature pyrolysis of magnetic nanoparticle and application.Described device is made up of material mixing pretreatment electrically heated reactor and multiple parallel electrical heating temperature-programmed reaction devices, and controls their reaction temperature and time simultaneously by a programmed temperature-rising controller.The device can be used for high temperature pyrolytic cracking (HTP) batch and prepare ferrite magnetic nano particle, such as ferroso-ferric oxide, Zn ferrite, manganese-zinc ferrite.It is parallel that the method passes through multiple reactors, and it is high successfully to solve high temperature pyrolytic cracking (HTP) reaction temperature, directly amplifies volume and prepares and there are problems that heat and mass is uneven, it is inhomogenous to be easily caused nanoparticle size.Reaction mass unification pretreatment and consolidator temperature control, it is ensured that reaction condition uniformity, can obtain high-quality magnetic nanoparticle.
Description
Technical field
The present invention relates to device prepared by a kind of parallel high temperature pyrolysis of magnetic nanoparticle, metal nanometer material preparation field.
Technical background
Magnetic ferrite nano particles are the nano materials that a class has specific function.Due to its special physical chemistry
Matter (such as small-size effect, skin effect), magnetism characteristic (such as superparamagnetism) and good biocompatibility, cure in biology
Magnetic resonance imaging, tumour magnetic induction thermotherapy, magnetic target medicine carrier, cell and bio-molecular separation and bio-sensing on
The fields such as detection have a wide range of applications.
In general, the field such as biomedicine is to the physicochemical properties of magnetic Nano structure, such as chemical composition, particle diameter,
Pattern, crystalline structure, magnetic property, homogeneity and dispersiveness etc. suffer from strict requirements.Therefore, high performance magnetic is prepared to receive
Prepared by rice grain, especially batch, to ensuring that biomedical applications are extremely important.Classical synthesis several at present
Method is including chemical coprecipitation, high temperature pyrolytic cracking (HTP), solvent-thermal method, microemulsion method and sol-gel process etc..Research shows, changes
It is current widely used two kinds of synthetic methods to learn coprecipitation and high temperature pyrolytic cracking (HTP).Wherein, chemical coprecipitation due to
Its preparation process is simple, equipment and raw material is relatively inexpensive, condition is easy to control, synthesis cycle is short, therefore can be used for magnetic Nano material
Batch prepare.But coprecipitation is generally difficult to obtain the good monodisperse magnetic nano particle of crystallinity, and receiving of obtaining
There is certain gap in rice grain saturation magnetization, be not prepare high performance magnetic nano material optimal compared with body phase material
Method.Comparatively speaking, high temperature pyrolytic cracking (HTP) is a kind of can to obtain preferable monodispersity, stability and crystallinity nano material
Common method, it is that in the presence of surfactants, heat resolve organo-metallic compound is (such as in high boiling organic solvent：
Metal acetylacetonate complex (M (acac) n, M=Fe, Mn, Co, Ni, Cr；N=2,3), metal carbonyl (M (CO) n)
A kind of method of nano particle is prepared with metal fatty acid salt.Although high-performance magnetism can be prepared by simply treating different things alike
Property nano particle, but because reaction temperature is high, when carrying out batch by simple volume iodine and preparing, exist serious
Heating heterogeneity, reaction system heat and mass heterogeneity causes the magnetic nanoparticles size for preparing to be distributed wide, between batch
Uniformity is poor, and magnetic property is unstable, it is difficult to meet the requirement of biomedical applications.Therefore, the warm high of development new model is needed badly
Solution batch prepares high performance magnetic nano particle.
The content of the invention
The invention aims to solve, heat and mass is uneven, be easily caused nanometer in prepared by high temperature pyrolytic cracking (HTP) amplification
Particle size heterogeneity, batch between uniformity difference problem.
For achieving the above object, the present invention is adopted the following technical scheme that：
1. the device that prepared by a kind of parallel high temperature pyrolysis of magnetic nanoparticle, it includes that material mixing pretreatment electrical heating is anti-
Device and multiple parallel electrical heating temperature-programmed reaction devices are answered, and their reaction is controlled by a programmed temperature-rising controller simultaneously
Temperature and time.
2. the device that prepared by the parallel high temperature pyrolysis of magnetic nanoparticle according to claim 1, it is characterised in that thing
Material mixing preatreating reactors capacity 0.5-5L, is controlled by electric heater unit linker warm-up controller and thermocouple
Temperature, and it is equipped with mechanical agitation and nitrogen is passed through pipeline.
3. the device that prepared by the parallel high temperature pyrolysis of magnetic nanoparticle according to claim 1, it is characterised in that by
Material mixing preatreating reactors material out respectively enters multiple parallel electrical heating temperature-programmed reaction devices, each electrical heating
Reactor all carries out the control of reaction temperature and time by same programmed temperature-rising controller and different thermocouples, and is equipped with cold
Solidifying pipe and nitrogen are passed through pipeline.
4. the device that prepared by the parallel high temperature pyrolysis of magnetic nanoparticle according to claim 1, it is characterised in that journey
Sequence warm-up controller is equipped with multiple thermocouples, can simultaneously control multiple electrically heated reactors.
5. the device that prepared by a kind of parallel high temperature pyrolysis of magnetic nanoparticle, it is characterised in that can be used for high temperature pyrolytic cracking (HTP) batch
Amount prepares ferrite magnetic nano particle, and concrete application step is as follows：
(1) 0.2-2L higher boiling reaction dissolvents are added in material mixing preatreating reactors, is continually fed into nitrogen to go
Except the oxygen in system；Add 20-200mmol ferric acetyl acetonade and different mol ratio oleic acid and oleyl amine (10: 0 to 0: 10,
Total amount is 120-1200mmol), under the conditions of nitrogen is passed through, by temperature programmed control device with 2-10 DEG C/min heating rates
To 100-120 DEG C, fully to remove more lower boiling water and impurity in solution, while so that acetyl acetone complex and oleic acid,
Oleyl amine mixing is complete, and keeps temperature 0.5-2h；
(2) material through material mixing preatreating reactors out, multiple parallel electricity are added separately to by liquid distributing device
Heating schedule temperature reaction device, feeding quantity 0.04-0.2L in each reactor is then arrived with 2-10 DEG C/min heating rates
200-230 DEG C (nucleation temperature) simultaneously maintains 0-2h；Continue to be warming up to 290-320 DEG C of (growth temperature with the 2-10 DEG C/min rates of heat addition
Degree), and 0.5-2h is stopped fully to complete the growth of nano particle, the temperature programmed control device controls the anti-of multiple reactors simultaneously
Answer temperature and time；
(3) after reaction terminates, thermal source is removed, unification is transferred in large beaker after naturally cooling to room temperature, adds anhydrous second
Alcohol or acetone, Magneto separate carry out the impurity such as washing 3-4 times, oleic acid, oleyl amine, the solvent remained in removal solution, are finally scattered in
Isooctane (or chloroform, hexamethylene etc.) middle preservation.
Beneficial effect
The present invention by material mix pretreatment electrically heated reactor, multiple electrical heating temperature-programmed reaction device parallel and
Unified programmed temperature-rising controller realizes prepared by the high temperature pyrolytic cracking (HTP) batch of magnetic nanoparticle.The method passes through multiple reactors
Parallel, successfully solve high temperature pyrolytic cracking (HTP) reaction temperature high, directly amplify volume and prepare and have that heat and mass is uneven, be easily caused
The inhomogenous problem of nanoparticle size.Reaction mass unification pretreatment and consolidator temperature control, it is ensured that reaction condition is consistent
Property, high-quality magnetic nanoparticle can be obtained.The device can be used for high temperature pyrolytic cracking (HTP) batch and prepare ferrite magnetic nano particle,
Such as ferroso-ferric oxide, Zn ferrite, manganese-zinc ferrite, highest design theory yield is about 23g ferrites, consistent with product
Property is good, size uniformity the advantages of.
Feature in aspects above of the present invention can independent assortment within the scope of the invention, as long as the technology after combination
Scheme falls in connotation of the invention, and application method is not limited by its order.
Brief description of the drawings
Device prepared by the parallel high temperature pyrolysis of Fig. 1 magnetic nanoparticles
(1. programmed temperature-rising controller；2. thermocouple line；3. electric heater；4. reactor；5. condenser pipe；6. nitrogen tube
Road；7. thermocouple；8. mechanical agitator；9. discharge pipe)
The parallel electrically heated reactor devices of Fig. 2 .5 100mL prepare the electromicroscopic photograph of manganese-zinc ferrite magnetic nano particle,
Oleic acid and oleyl amine mol ratio are respectively (A) 10: 2, (B) 7: 5, (C) 5: 7
The parallel electrically heated reactor devices of Fig. 3 .5 250mL prepare the electromicroscopic photograph (A) of zinc ferrite magnetic nano particle
And its size distribution plot (B)
The parallel electrically heated reactor devices of Fig. 4 .10 500mL prepare ferroferric oxide magnetic nanoparticle electromicroscopic photograph
(A), size distribution plot (B), and electron diffraction diagram (C)
Specific embodiment：
Below in conjunction with the accompanying drawings and specific embodiment, the present invention is furture elucidated, it should be understood that these implementation methods are only used for
The bright present invention rather than limitation the scope of the present invention, after reading this disclosure, those skilled in the art is to of the invention
The modification of the various equivalent form of values falls within claims hereof limited range.
The device that in the present invention prepared by the parallel high temperature pyrolysis of magnetic nanoparticle is reacted by material mixing pretreatment electrical heating
Device and multiple parallel electrical heating temperature-programmed reaction device compositions, and the anti-of them is controlled by a programmed temperature-rising controller simultaneously
Answer temperature and time.Device is as shown in figure 1, including following part：1. programmed temperature-rising controller；2. thermocouple line；3. electricity adds
Hot device；4. reactor；5. condenser pipe；6. nitrogen pipeline；7. thermocouple；8. mechanical agitator；9. discharge pipe.
1,5 parallel electrically heated reactor devices of 100mL of embodiment prepare manganese-zinc ferrite magnetic nano particle
Preparation facilities is by 0.5L materials mixing pretreatment electrically heated reactor, 5 parallel electrical heating temperature-programmed reaction devices
(0.1L) and 1 programmed temperature-rising controller composition.Preparation process is as follows：
(1) 0.2L dioctyl ethers are added in material mixing preatreating reactors, is continually fed into nitrogen with removal system
Oxygen；Add ferric acetyl acetonade, the manganese acetylacetonate of 6mmol, the zinc acetylacetonate of 4mmol and the different mol ratio of 20mmol
Oleic acid and oleyl amine (respectively 10: 2,7: 5,5: 7, total amount is 120mmol), under the conditions of nitrogen is passed through, by temperature programmed control
Device with 3 DEG C/min heating rates to 110 DEG C, fully to remove more lower boiling water and impurity in solution, while so that
Acetyl acetone complex and oleic acid, oleyl amine mixing completely, and keep temperature 1h.
(2) material through material mixing preatreating reactors out, is added separately to 5 parallel electricity and adds by liquid distributing device
Hot temperature-programmed reaction device, feeding quantity 0.04L in each reactor, then with 3 DEG C/min heating rates to 220 DEG C (into
Nuclear temperature) and maintain 2h；Continuation is warming up to 300 DEG C (growth temperatures) with the 3 DEG C/min rates of heat addition, and stops 1h fully to complete
The growth of nano particle.
(3) after reaction terminates, thermal source is removed, unification is transferred in beaker after naturally cooling to room temperature, adds absolute ethyl alcohol,
Magneto separate carries out washing 3-4 times, oleic acid, the oleyl amine remained in removal solution.Acetone is added, two remained in removal solution are pungent
Be scattered in magnetic nanoparticle in isooctane after carrying out washing 2 times preserve by ether, Magneto separate.
2.1g manganese-zinc ferrite magnetic nano particles, yield about 90% can obtain by above-mentioned preparation facilities.The magnetic for obtaining
Property nanoparticle size is homogeneous, and can obtain the nanometer of different sizes and shapes by controlling the ratio of oleic acid and oleyl amine
Particle, as shown in Figure 2.Specifically, when the mol ratio of oleic acid and oleyl amine is 10: 2, the spherical nanoparticle of pattern rule is obtained
(9nm)；And the mol ratio for working as oleic acid and oleyl amine is when being 7: 5 and 5: 7, obtain be monodispersity Cubic nano particle (11nm)
With star nano particle (16nm).
2,5 parallel electrically heated reactor devices of 250mL of embodiment prepare zinc ferrite magnetic nano particle
Preparation facilities is by 1L materials mixing pretreatment electrically heated reactor, 5 parallel electrical heating temperature-programmed reaction devices
(0.25L) and 1 programmed temperature-rising controller composition.Preparation process is as follows：
(1) 0.5L benzyl ether is added in material mixing preatreating reactors, is continually fed into nitrogen with removal system
Oxygen；Ferric acetyl acetonade, the zinc acetylacetonate of 90mmol and the 700mmol oleic acid of 180mmol are added, condition is passed through in nitrogen
Under, by temperature programmed control device with 8 DEG C/min heating rates to 120 DEG C, fully to remove more lower boiling water in solution
And impurity, while so that acetyl acetone complex and oleic acid, oleyl amine mixing completely, and keep temperature 1h.
(2) material through material mixing preatreating reactors out, is added separately to 5 parallel electricity and adds by liquid distributing device
Hot temperature-programmed reaction device, feeding quantity 0.1L in each reactor, then with 8 DEG C/min heating rates to 290 DEG C of (growths
Temperature), and 1h is stopped fully to complete the growth of nano particle.
(3) after reaction terminates, thermal source is removed, unification is transferred in beaker after naturally cooling to room temperature, adds absolute ethyl alcohol,
Magneto separate carries out the impurity such as washing 3-4 times, oleic acid, oleyl amine, the benzyl ether remained in removal solution, finally by magnetic nanoparticle
It is scattered in preservation in chloroform.
About 12g zinc ferrite magnetic nano particles, yield about 86% can be obtained by above-mentioned preparation facilities.The magnetic for obtaining
Nanoparticle size is homogeneous, subsphaeroidal, average-size 17nm, as shown in Figure 3.
3,10 parallel electrically heated reactor devices of 500mL of embodiment prepare ferroferric oxide magnetic nanoparticle
Preparation facilities is by 5L materials mixing pretreatment electrically heated reactor, 10 parallel electrical heating temperature-programmed reaction devices
(0.5L) and 1 programmed temperature-rising controller composition.Preparation process is as follows：
(1) 2L benzyl ether is added in material mixing preatreating reactors, is continually fed into nitrogen with the oxygen in removal system
Gas；The ferric acetyl acetonade of 300mmol and the oleic acid and oleyl amine (total amount is 1200mmol) of 10: 2 mol ratios are added, it is logical in nitrogen
It is relatively low in solution fully to remove by temperature programmed control device with 3.3 DEG C/min heating rates to 110 DEG C under the conditions of entering
The water and impurity of boiling point, while so that acetyl acetone complex and oleic acid, oleyl amine mixing completely, and keep temperature 1h.
(2) material through material mixing preatreating reactors out, 10 parallel electricity are added separately to by liquid distributing device
Heating schedule temperature reaction device, feeding quantity 0.2L in each reactor, then with 3.3 DEG C/min heating rates to 220 DEG C
(nucleation temperature) and maintain 1h；Continuation is warming up to 290 DEG C (growth temperatures) with the 3.3 DEG C/min rates of heat addition, and stops 1h to fill
Divide the growth for completing nano particle.
(3) after reaction terminates, thermal source is removed, unification is transferred in beaker after naturally cooling to room temperature, adds absolute ethyl alcohol,
Magneto separate carries out the impurity such as washing 3-4 times, oleic acid, oleyl amine, the benzyl ether remained in removal solution, finally by magnetic nanoparticle
It is scattered in preservation in n-hexane.
About 20g manganese-zinc ferrite magnetic nano particles, yield about 86% can be obtained by above-mentioned preparation facilities.The magnetic for obtaining
Property nanoparticle size is homogeneous, subsphaeroidal, average-size 15nm, with cubic spinel structure, as shown in Figure 4.
Claims (5)
1. the device that prepared by a kind of parallel high temperature pyrolysis of magnetic nanoparticle, it includes material mixing pretreatment electrically heated reactor
With multiple parallel electrical heating temperature-programmed reaction devices, and their reaction temperature is controlled by a programmed temperature-rising controller simultaneously
And the time.
2. the device that prepared by the parallel high temperature pyrolysis of magnetic nanoparticle according to claim 1, it is characterised in that material is mixed
Preatreating reactors capacity 0.5-5L is closed, temperature control is carried out by electric heater unit linker warm-up controller and thermocouple, and
It is equipped with mechanical agitation and nitrogen is passed through pipeline.
3. the device that prepared by the parallel high temperature pyrolysis of magnetic nanoparticle according to claim 1, it is characterised in that by material
Mixing preatreating reactors material out respectively enters multiple parallel electrical heating temperature-programmed reaction devices, each electrical heating reaction
Device all carries out the control of reaction temperature and time by same programmed temperature-rising controller and different thermocouples, and is equipped with condenser pipe
Pipeline is passed through with nitrogen.
4. the device that prepared by the parallel high temperature pyrolysis of magnetic nanoparticle according to claim 1, it is characterised in that program liter
Temperature controller is equipped with multiple thermocouples, can simultaneously control multiple electrically heated reactors.
5. the device that prepared by a kind of parallel high temperature pyrolysis of magnetic nanoparticle, it is characterised in that can be used for high temperature pyrolytic cracking (HTP) batch and make
Standby ferrite magnetic nano particle, concrete application step is as follows：
(1) 0.2-2L higher boiling reaction dissolvents are added in material mixing preatreating reactors, is continually fed into nitrogen with removing body
Oxygen in system；Add the ferric acetyl acetonade of 20-200mmol and oleic acid and oleyl amine (10: 0 to 0: 10, total amount of different mol ratio
It is 120-1200mmol), under the conditions of nitrogen is passed through, arrived with 2-10 DEG C/min heating rates by temperature programmed control device
100-120 DEG C, fully to remove more lower boiling water and impurity in solution, while so that acetyl acetone complex and oleic acid, oil
Amine mixing is complete, and keeps temperature 0.5-2h；
(2) material through material mixing preatreating reactors out, multiple parallel electrical heating are added separately to by liquid distributing device
Temperature-programmed reaction device, feeding quantity 0.04-0.2L in each reactor, then with 2-10 DEG C/min heating rates to 200-
230 DEG C (nucleation temperatures) simultaneously maintain 0-2h；Continuation is warming up to 290-320 DEG C (growth temperature) with the 2-10 DEG C/min rates of heat addition,
And 0.5-2h is stopped fully to complete the growth of nano particle, the temperature programmed control device controls the reaction temperature of multiple reactors simultaneously
Degree and time；
(3) after reaction terminates, remove thermal source, naturally cool to unification after room temperature and be transferred in large beaker, add absolute ethyl alcohol or
Acetone, Magneto separate carries out the impurity such as washing 3-4 times, oleic acid, oleyl amine, the solvent remained in removal solution, is finally scattered in different pungent
Alkane (or chloroform, hexamethylene etc.) middle preservation.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108578697A (en) * | 2018-05-17 | 2018-09-28 | 桂林医学院附属医院 | A kind of preparation method of chlorin e 6 and ferroso-ferric oxide composite nanoparticle |
| CN108806960A (en) * | 2018-04-24 | 2018-11-13 | 沈阳工业大学 | A kind of liquid phase chemical combination method preparing Nd-Fe-B permanent magnetic nano-particle |
| CN111732127A (en) * | 2020-07-02 | 2020-10-02 | 安徽大学 | Method for thermally synthesizing ferrite by magnetic field auxiliary solvent and method for regulating and controlling size and morphological characteristics of magnetic grains |
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| CN103449530A (en) * | 2013-09-06 | 2013-12-18 | 南京东纳生物科技有限公司 | Preparation method of high-performance magnetic manganese zinc ferrite nanostars and nanoclusters |
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| CN205462321U (en) * | 2016-03-09 | 2016-08-17 | 杭州老桐君制药有限公司 | Even arrange condensing reflux device |
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| CN2581065Y (en) * | 2002-11-27 | 2003-10-22 | 中国铝业股份有限公司 | Water-bath stirring reaction tank |
| CN202113857U (en) * | 2011-05-30 | 2012-01-18 | 中国科学院广州能源研究所 | Novel oil bath type fully-mixed-flow miniature reaction equipment |
| CN103449530A (en) * | 2013-09-06 | 2013-12-18 | 南京东纳生物科技有限公司 | Preparation method of high-performance magnetic manganese zinc ferrite nanostars and nanoclusters |
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| CN108806960A (en) * | 2018-04-24 | 2018-11-13 | 沈阳工业大学 | A kind of liquid phase chemical combination method preparing Nd-Fe-B permanent magnetic nano-particle |
| CN108806960B (en) * | 2018-04-24 | 2020-07-17 | 沈阳工业大学 | Liquid phase combination method for preparing neodymium iron boron permanent magnetic nano particles |
| CN108578697A (en) * | 2018-05-17 | 2018-09-28 | 桂林医学院附属医院 | A kind of preparation method of chlorin e 6 and ferroso-ferric oxide composite nanoparticle |
| CN111732127A (en) * | 2020-07-02 | 2020-10-02 | 安徽大学 | Method for thermally synthesizing ferrite by magnetic field auxiliary solvent and method for regulating and controlling size and morphological characteristics of magnetic grains |
| CN111732127B (en) * | 2020-07-02 | 2022-04-19 | 安徽大学 | Method for thermally synthesizing ferrite by magnetic field auxiliary solvent and method for regulating and controlling size and morphological characteristics of magnetic grains |
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Application publication date: 20170531 |