CN108996550A - MFe2O4Nanometer particle congery and preparation method thereof - Google Patents
MFe2O4Nanometer particle congery and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of MFe2O4(M=Mn, Co or Ni) nanometer particle congery, it the preparation method comprises the following steps: 65 ~ 120 mM, 1 mL alkane bromination ammonium 1) is added to 1 mL MFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 5 ~ 15 minutes under 38 ~ 42 DEG C of water bath conditions, and the high molecular ethylene glycol solution of 5 mL, 2 mM is added, 75 ~ 85 DEG C are heated under nitrogen protection, stirs 5 ~ 7 hours, is cooled to room temperature；2) centrifuge washing obtains MFe2O4Nanometer particle congery；The invention has the following advantages that 1, preparation method is simple, and it is reproducible, it is suitble to investment actual production；2, by adjusting the response parameters such as alkane bromination ammonium specy and additional amount, it can be achieved that MFe2O4The accuracy controlling of (M=Mn, Co or Ni) nanometer particle congery size；3, the MFe prepared2O4(M=Mn, Co or Ni) nanometer particle congery, which has, is better than MFe2O4The light thermal property of nanoparticle can be applied to the fields such as photo-thermal therapy, magnetic resonance imaging and bio-separation.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to MFe2O4Nanometer particle congery and its preparation side
Method.
Background technique
In recent years, world's cancer morbidity rises year by year, and morbidity crowd's average age declines year by year, and treatment of cancer problem is carved
Do not allow to delay.Traditional anti-cancer therapies are mainly operative treatment, radiation cure and chemotherapy, and main problem is to swollen
The damage that normal tissue is easily caused when tumor tissue is treated, the wound after treatment is big and is easy recurrence.
The appearance of photo-thermal therapy method is that treatment of cancer is filled with new vitality, and principle is close red using light thermit powder absorption
Outer light generates heat, and tumour cell is made to be warming up to 42 DEG C or more in a short time, causes irreversible killing to imitate tumor tissues
Fruit.The advantages of method of this treating cancer is that fixed point ablation can be realized to tumour cell, reduces the damage to normal cell；
Easy to operate, seance process only needs a few minutes that can complete；It brings pain small to patient, no wound may be implemented and control
It treats.
The numerous areas such as superparamagnetic nanoparticle transports in bio-separation, immune detection, drug targeting, Magnetic resonance imaging
It is with a wide range of applications, is one of the hot spot of current field of nanometer material technology research.There is researcher's discovery in recent years
MnFe2O4Superparamagnetic nanoparticle has light thermal property, realized while can be used for photo-thermal therapy Magnetic resonance imaging and heat at
Picture.How to optimize and improve MnFe2O4The Nomenclature Composition and Structure of Complexes of nanometer photo-thermal therapy agent, enhances its near infrared absorption, improves its photo-thermal
Performance develops its multifunctionality, more efficient treatment of cancer effect is obtained under conditions of ensureing biological safety, is still one
The research topic of great challenge.It is to improve one of the effective way of material self performance that nanoparticle, which is carried out regulation arrangement,.Have
Nanoparticle is assembled into chain or nanometer particle congery structure by research report facilitates being optimal of electronic structure, in turn
Significantly improve its physical and chemical performance.MnFe2O4Near infrared absorption be derived mainly from the electric charge transfer between valence, received if assembled them into
Rice corpuscles aggregation, then the interaction between metal ion will become by force, near infrared absorption will enhance, and light thermal property also can
It improves.Meanwhile the Brillouin Zone Folding effect that self-assembled structures cause can also make certain sub-band transitions prohibited by selection rule
It is lifted a ban, enhances near infrared absorption, improve light thermal property.In addition, CoFe2O4、NiFe2O4Equal superparamagnetic nanomaterials exist
There is also certain absorptions near infrared region, but at present it is not yet found that the report of its light thermal property is developed, more without proposing to pass through
Its nanoparticle aggregation is constructed to improve the design philosophy of light thermal property, therefore is researched and developed a kind of with superparamagnetism and light thermal property
MFe2O4(M=Mn, Co or Ni) nanoparticle aggregation and preparation method thereof is significant.
Summary of the invention
The object of the present invention is to provide a kind of MFe for having both superparamagnetism and light thermal property2O4(M=Mn, Co or Ni) nanometer
Particle agglomeration and preparation method thereof.
MFe2O4The preparation method of nanometer particle congery, it includes:
1) the alkane bromination ammonium that 1mL concentration is 65 ~ 120mM is added to the MFe of 1mL2O4In nanoparticle chloroformic solution, 38 ~
Nitrogen is passed through 5 ~ 15 minutes under 42 DEG C of water bath conditions, and the high molecular ethylene glycol solution that 5mL concentration is 2mM, nitrogen protection is added
Under be heated to 75 ~ 85 DEG C, stir 5 ~ 7 hours, be cooled to room temperature；
2) centrifuge washing obtains MFe2O4Nanometer particle congery；
MFe described in step 1)2O4Nanoparticle is the MnFe with oleic acid and oily ammonium modification2O4、CoFe2O4Or NiFe2O4Nanoparticle
Son；
The MFe2O4Nanoparticle is prepared by the following method:
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and acetyl acetone salt that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C
And constant temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；It is washed under magnet help with ethyl alcohol
It washs 3 times, obtains MFe2O4Nanoparticle；
The acetyl acetone salt is manganese acetylacetonate, acetylacetone cobalt or nickel acetylacetonate；
Alkane bromination ammonium described in step 1) is dodecyl trimethyl ammonium bromide, tetradecyltrimethylammonium bromide or hexadecane
Base trimethylammonium bromide；
Macromolecule described in step 1) is polyvinylpyrrolidone, polyethyleneimine, polyacrylic acid or kayexalate；
Nanoparticle chloroformic solution concentration described in step 1) is 20 mg/mL.
MFe2O4Nanometer particle congery, it is prepared by the above method.
MFe2O4Purposes of the nanometer particle congery in terms of light thermal property.
MFe2O4Application of the nanometer particle congery in photo-thermal therapy instrument, magnetic resonance imaging and bio-separation.
The present invention provides MFe2O4(M=Mn, Co or Ni) nanometer particle congery, it is prepared by the following method: 1)
65 ~ 120 mM, 1 mL alkane bromination ammonium is added to 1 mL MFe2O4In nanoparticle chloroformic solution, 38 ~ 42 DEG C of water bath conditions
Under be passed through nitrogen 5 ~ 15 minutes, the high molecular ethylene glycol solution of 5 mL, 2 mM is added, is heated to 75 ~ 85 DEG C under nitrogen protection, stirs
It mixes 5 ~ 7 hours, is cooled to room temperature；2) centrifuge washing obtains MFe2O4Nanometer particle congery；The invention has the following advantages that 1,
Preparation method is simple, reproducible, is suitble to investment actual production；2, by adjusting the reaction such as alkane bromination ammonium specy and additional amount
Parameter is, it can be achieved that MFe2O4The accuracy controlling of (M=Mn, Co or Ni) nanometer particle congery size；3, the MFe prepared2O4(M=
Mn, Co or Ni) nanometer particle congery have be better than MFe2O4It is total to can be applied to photo-thermal therapy, magnetic for the light thermal property of nanoparticle
The fields such as vibration imaging and bio-separation.
Detailed description of the invention
Fig. 1 is polyvinyl pyrrolidon modified MnFe2O4The scanning electron microscope (SEM) photograph of nanometer particle congery；
Fig. 2 is MFe2O4Nanometer particle congery size and alkane bromination ammonium specy relationship histogram；
Fig. 3 is MFe2O4Magnitude relation histogram is added in nanometer particle congery size and dodecyl trimethyl ammonium bromide；
Fig. 4 is MnFe under 808 nm laser irradiations2O4Nanoparticle, MnFe2O4The heating curve of nanometer particle congery and water.
Specific embodiment
The MnFe that 1 oleic acid of embodiment, oily ammonium are modified2O4The preparation of nanoparticle
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and manganese acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；Ethanol washing 3 is used under magnet help
It is secondary, obtain the MnFe that size is about 7 nm2O4Nanoparticle.
The CoFe that 2 oleic acid of embodiment, oily ammonium are modified2O4The preparation of nanoparticle
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and acetylacetone cobalt that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；Ethanol washing 3 is used under magnet help
It is secondary, obtain the CoFe that size is about 10 nm2O4Nanoparticle.
The NiFe that 3 oleic acid of embodiment, oily ammonium are modified2O4The preparation of nanoparticle
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and nickel acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；Ethanol washing 3 is used under magnet help
It is secondary, obtain the NiFe that size is about 9 nm2O4Nanoparticle.
The polyvinyl pyrrolidon modified MnFe of embodiment 42O4The preparation of nanometer particle congery
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and manganese acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；With washing 3 times under magnet help, obtain
Obtain the monodisperse MnFe of 20 mg/mL2O4Nanoparticle；65 mM, 1 mL dodecyl trimethyl ammonium bromide aqueous solution is added to
1 mL MnFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 10 minutes under 40 DEG C of water bath conditions, and the poly- second of 2 mM, 5 mL is added
Alkene pyrrolidone ethylene glycol solution is heated to 80 DEG C under nitrogen protection, stirs 6 hours, is cooled to room temperature；Centrifuge washing three times,
Obtain the MnFe that polyvinyl pyrrolidon modified size is about 300 nm2O4Nanometer particle congery；Polyvinylpyrrolidone is repaired
The MnFe of decorations2O4The scanning electron microscope (SEM) photograph of nanometer particle congery is shown in Fig. 1.
The polyvinyl pyrrolidon modified CoFe of embodiment 52O4The preparation of nanometer particle congery
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and at 80 DEG C
Under stir to clarify；The ferric acetyl acetonade and acetylacetone cobalt that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and constant temperature
1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；It is used ethanol washing 3 times under magnet help,
Obtain the monodisperse CoFe of 20 mg/mL2O4Nanoparticle；65 mM, 1 mL dodecyl trimethyl ammonium bromide aqueous solution is added
To 1 mL CoFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 10 minutes under 40 DEG C of water bath conditions, and it is poly- that 2 mM, 5 mL is added
Vinylpyrrolidone ethylene glycol solution is heated to 80 DEG C under nitrogen protection, stirs 6 hours, is cooled to room temperature；Centrifuge washing three
Time, obtain the CoFe that polyvinyl pyrrolidon modified size is about 320 nm2O4Nanometer particle congery.
The polyvinyl pyrrolidon modified NiFe of embodiment 62O4The preparation of nanometer particle congery
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and at 80 DEG C
Under stir to clarify；The ferric acetyl acetonade and nickel acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and constant temperature
1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；It is used ethanol washing 3 times under magnet help,
Obtain the monodisperse NiFe of 20 mg/mL2O4Nanoparticle；65 mM, 1 mL dodecyl trimethyl ammonium bromide aqueous solution is added
To 1 mL NiFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 10 minutes under 40 DEG C of water bath conditions, and it is poly- that 2 mM, 5 mL is added
Vinylpyrrolidone ethylene glycol solution is heated to 80 DEG C under nitrogen protection, stirs 6 hours, is cooled to room temperature；Centrifuge washing three
Time, obtain the NiFe that polyvinyl pyrrolidon modified size is about 310 nm2O4Nanometer particle congery.
The polyvinyl pyrrolidon modified MnFe of embodiment 72O4The preparation of nanometer particle congery
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and manganese acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；With washing 3 times under magnet help, obtain
Obtain the monodisperse MnFe of 20 mg/mL2O4Nanoparticle；90 mM, 1 mL dodecyl trimethyl ammonium bromide aqueous solution is added to
1 mL MnFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 10 minutes under 40 DEG C of water bath conditions, and the poly- second of 2 mM, 5 mL is added
Alkene pyrrolidone ethylene glycol solution is heated to 80 DEG C under nitrogen protection, stirs 6 hours, is cooled to room temperature；Centrifuge washing three times,
Obtain the MnFe that polyvinyl pyrrolidon modified size is about 250 nm2O4Nanometer particle congery.
The polyvinyl pyrrolidon modified MnFe of embodiment 82O4The preparation of nanometer particle congery
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and manganese acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；With washing 3 times under magnet help, obtain
Obtain the monodisperse MnFe of 20 mg/mL2O4Nanoparticle；120 mM, 1 mL dodecyl trimethyl ammonium bromide aqueous solution is added
To 1 mL MnFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 10 minutes under 40 DEG C of water bath conditions, and it is poly- that 2 mM, 5 mL is added
Vinylpyrrolidone ethylene glycol solution is heated to 80 DEG C under nitrogen protection, stirs 6 hours, is cooled to room temperature；Centrifuge washing three
Time, obtain the MnFe that polyvinyl pyrrolidon modified size is about 220 nm2O4Nanometer particle congery.
The polyvinyl pyrrolidon modified MnFe of embodiment 92O4The preparation of nanometer particle congery
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and manganese acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；With washing 3 times under magnet help, obtain
Obtain the monodisperse MnFe of 20 mg/mL2O4Nanoparticle；65 mM, 1 mL tetradecyltrimethylammonium bromide aqueous solution is added to
1 mL MnFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 10 minutes under 40 DEG C of water bath conditions, and the poly- second of 2 mM, 5 mL is added
Alkene pyrrolidone ethylene glycol solution is heated to 80 DEG C under nitrogen protection, stirs 6 hours, is cooled to room temperature；Centrifuge washing three times,
Obtain the MnFe that polyvinyl pyrrolidon modified size is about 280 nm2O4Nanometer particle congery.
The polyvinyl pyrrolidon modified MnFe of embodiment 102O4The preparation of nanometer particle congery
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and manganese acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；With washing 3 times under magnet help, obtain
Obtain the monodisperse MnFe of 20 mg/mL2O4Nanoparticle；65 mM, 1 mL cetyl trimethylammonium bromide aqueous solution is added to
1 mL MnFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 10 minutes under 40 DEG C of water bath conditions, and the poly- second of 2 mM, 5 mL is added
Alkene pyrrolidone ethylene glycol solution is heated to 80 DEG C under nitrogen protection, stirs 6 hours, is cooled to room temperature；Centrifuge washing three times,
Obtain the MnFe that polyvinyl pyrrolidon modified size is about 220 nm2O4Nanometer particle congery.
The amine-modified MnFe of 11 polyethyleneimine of embodiment2O4The preparation of nanometer particle congery
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and manganese acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；With washing 3 times under magnet help, obtain
Obtain the monodisperse MnFe of 20 mg/mL2O4Nanoparticle；65 mM, 1 mL dodecyl trimethyl ammonium bromide aqueous solution is added to
1 mL MnFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 10 minutes under 40 DEG C of water bath conditions, and the poly- second of 2 mM, 5 mL is added
Alkene imines ethylene glycol solution is heated to 80 DEG C under nitrogen protection, stirs 6 hours, is cooled to room temperature；It centrifuge washing three times, obtains
The MnFe that the amine-modified size of polyethyleneimine is about 290 nm2O4Nanometer particle congery.
The MnFe of 12 polyacrylic acid of embodiment modification2O4The preparation of nanometer particle congery
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and manganese acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；With washing 3 times under magnet help, obtain
Obtain the monodisperse MnFe of 20 mg/mL2O4Nanoparticle；65 mM, 1 mL dodecyl trimethyl ammonium bromide aqueous solution is added to
1 mL MnFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 10 minutes under 40 DEG C of water bath conditions, and 2 mM, 5 mL poly- third is added
Olefin(e) acid ethylene glycol solution is heated to 80 DEG C under nitrogen protection, stirs 6 hours, is cooled to room temperature；Centrifuge washing three times, gathered
The MnFe that the size of acrylic acid modification is about 300 nm2O4Nanometer particle congery.
The MnFe of 13 kayexalate of embodiment modification2O4The preparation of nanometer particle congery
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and manganese acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；With washing 3 times under magnet help, obtain
Obtain the monodisperse MnFe of 20 mg/mL2O4Nanoparticle；65 mM, 1 mL dodecyl trimethyl ammonium bromide aqueous solution is added to
1 mL MnFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 10 minutes under 40 DEG C of water bath conditions, and 2 mM, 5 mL polyphenyl is added
Vinyl sulfonic acid sodium ethylene glycol solution is heated to 80 DEG C under nitrogen protection, stirs 6 hours, is cooled to room temperature；Centrifuge washing three times,
Obtain the MnFe that the size of kayexalate modification is about 310 nm2O4Nanometer particle congery.
The polyvinyl pyrrolidon modified MnFe of embodiment 142O4The preparation of nanometer particle congery
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and manganese acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；With washing 3 times under magnet help, obtain
Obtain the monodisperse MnFe of 20 mg/mL2O4Nanoparticle；65 mM, 1 mL dodecyl trimethyl ammonium bromide aqueous solution is added to
1 mL MnFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 10 minutes under 40 DEG C of water bath conditions, and the poly- second of 2 mM, 5 mL is added
Alkene pyrrolidone ethylene glycol solution is heated to 75 DEG C under nitrogen protection, stirs 6 hours, is cooled to room temperature；Centrifuge washing three times,
Obtain the MnFe that polyvinyl pyrrolidon modified size is about 300 nm2O4Nanometer particle congery.
The polyvinyl pyrrolidon modified MnFe of embodiment 152O4The preparation of nanometer particle congery
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and manganese acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；With washing 3 times under magnet help, obtain
Obtain the monodisperse MnFe of 20 mg/mL2O4Nanoparticle；65 mM, 1 mL dodecyl trimethyl ammonium bromide aqueous solution is added to
1 mL MnFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 10 minutes under 40 DEG C of water bath conditions, and the poly- second of 2 mM, 5 mL is added
Alkene pyrrolidone ethylene glycol solution is heated to 85 DEG C under nitrogen protection, stirs 6 hours, is cooled to room temperature；Centrifuge washing three times,
Obtain the MnFe that polyvinyl pyrrolidon modified size is about 300 nm2O4Nanometer particle congery.
The polyvinyl pyrrolidon modified MnFe of embodiment 162O4The preparation of nanometer particle congery
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and manganese acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；With washing 3 times under magnet help, obtain
Obtain the monodisperse MnFe of 20 mg/mL2O4Nanoparticle；65 mM, 1 mL dodecyl trimethyl ammonium bromide aqueous solution is added to
1 mL MnFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 10 minutes under 40 DEG C of water bath conditions, and the poly- second of 2 mM, 5 mL is added
Alkene pyrrolidone ethylene glycol solution is heated to 80 DEG C under nitrogen protection, stirs 5 hours, is cooled to room temperature；Centrifuge washing three times,
Obtain the MnFe that polyvinyl pyrrolidon modified size is about 300 nm2O4Nanometer particle congery.
The polyvinyl pyrrolidon modified MnFe of embodiment 172O4The preparation of nanometer particle congery
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and manganese acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；With washing 3 times under magnet help, obtain
Obtain the monodisperse MnFe of 20 mg/mL2O4Nanoparticle；65 mM, 1 mL dodecyl trimethyl ammonium bromide aqueous solution is added to
1 mL MnFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 10 minutes under 40 DEG C of water bath conditions, and the poly- second of 2 mM, 5 mL is added
Alkene pyrrolidone ethylene glycol solution is heated to 80 DEG C under nitrogen protection, stirs 7 hours, is cooled to room temperature；Centrifuge washing three times,
Obtain the MnFe that polyvinyl pyrrolidon modified size is about 300 nm2O4Nanometer particle congery.
The polyvinyl pyrrolidon modified MnFe of embodiment 182O4The preparation of nanometer particle congery
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and manganese acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；With washing 3 times under magnet help, obtain
Obtain the monodisperse MnFe of 20 mg/mL2O4Nanoparticle；65 mM, 1 mL dodecyl trimethyl ammonium bromide aqueous solution is added to
1 mL MnFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 10 minutes under 38 DEG C of water bath conditions, and the poly- second of 2 mM, 5 mL is added
Alkene pyrrolidone ethylene glycol solution is heated to 80 DEG C under nitrogen protection, stirs 6 hours, is cooled to room temperature；Centrifuge washing three times,
Obtain the MnFe that polyvinyl pyrrolidon modified size is about 300 nm2O4Nanometer particle congery.
The polyvinyl pyrrolidon modified MnFe of embodiment 192O4The preparation of nanometer particle congery
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and manganese acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；With washing 3 times under magnet help, obtain
Obtain the monodisperse MnFe of 20 mg/mL2O4Nanoparticle；65 mM, 1 mL dodecyl trimethyl ammonium bromide aqueous solution is added to
1 mL MnFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 10 minutes under 42 DEG C of water bath conditions, and the poly- second of 2 mM, 5 mL is added
Alkene pyrrolidone ethylene glycol solution is heated to 80 DEG C under nitrogen protection, stirs 6 hours, is cooled to room temperature；Centrifuge washing three times,
Obtain the MnFe that polyvinyl pyrrolidon modified size is about 300 nm2O4Nanometer particle congery.
The polyvinyl pyrrolidon modified MnFe of embodiment 202O4The preparation of nanometer particle congery
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and manganese acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；With washing 3 times under magnet help, obtain
Obtain the monodisperse MnFe of 20 mg/mL2O4Nanoparticle；65 mM, 1 mL dodecyl trimethyl ammonium bromide aqueous solution is added to
1 mL MnFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 5 minutes under 40 DEG C of water bath conditions, and the poly- second of 2 mM, 5 mL is added
Alkene pyrrolidone ethylene glycol solution is heated to 80 DEG C under nitrogen protection, stirs 6 hours, is cooled to room temperature；Centrifuge washing three times,
Obtain the MnFe that polyvinyl pyrrolidon modified size is about 300 nm2O4Nanometer particle congery.
The polyvinyl pyrrolidon modified MnFe of embodiment 212O4The preparation of nanometer particle congery
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and manganese acetylacetonate that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C and perseverance
Temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；With washing 3 times under magnet help, obtain
Obtain the monodisperse MnFe of 20 mg/mL2O4Nanoparticle；65 mM, 1 mL dodecyl trimethyl ammonium bromide aqueous solution is added to
1 mL MnFe2O4In nanoparticle chloroformic solution, nitrogen is passed through 15 minutes under 40 DEG C of water bath conditions, and the poly- second of 2 mM, 5 mL is added
Alkene pyrrolidone ethylene glycol solution is heated to 80 DEG C under nitrogen protection, stirs 6 hours, is cooled to room temperature；Centrifuge washing three times,
Obtain the MnFe that polyvinyl pyrrolidon modified size is about 300 nm2O4Nanometer particle congery.
Claims (10)
1.MFe2O4The preparation method of nanometer particle congery, it includes:
1) the alkane bromination ammonium that 1mL concentration is 65 ~ 120mM is added to the MFe of 1mL2O4In nanoparticle chloroformic solution, 38 ~ 42
Nitrogen is passed through 5 ~ 15 minutes under DEG C water bath condition, is added the high molecular ethylene glycol solution that 5mL concentration is 2mM, under nitrogen protection
75 ~ 85 DEG C are heated to, stirs 5 ~ 7 hours, is cooled to room temperature；
2) centrifuge washing obtains MFe2O4Nanometer particle congery.
2. MFe according to claim 12O4The preparation method of nanometer particle congery, it is characterised in that: described in step 1)
MFe2O4Nanoparticle is the MnFe with oleic acid and oily ammonium modification2O4、CoFe2O4Or NiFe2O4Nanoparticle.
3. MFe according to claim 22O4The preparation method of nanometer particle congery, it is characterised in that: the MFe2O4
Nanoparticle is prepared by the following method:
The benzyl ether of the 1,2- hexadecane diol of 10 mM, the oleic acid of 2 mM, the oleyl amine of 2 mM and 20 mL are mixed and 80
It is stirred to clarify at DEG C；The ferric acetyl acetonade and acetyl acetone salt that molar ratio is respectively 1:1.5 is added, is warming up to 200 DEG C
And constant temperature 1 hour, then it is warming up to 300 DEG C and constant temperature 1 hour；End of reaction removes heat source；It is washed under magnet help with ethyl alcohol
It washs 3 times, obtains MFe2O4Nanoparticle.
4. MFe according to claim 32O4The preparation method of nanometer particle congery, it is characterised in that: the acetyl
Acetone metal salt is manganese acetylacetonate, acetylacetone cobalt or nickel acetylacetonate.
5. MFe according to claim 1,2,3 or 42O4The preparation method of nanometer particle congery, it is characterised in that: step
1) the alkane bromination ammonium described in is dodecyl trimethyl ammonium bromide, tetradecyltrimethylammonium bromide or cetyl trimethyl
Ammonium bromide.
6. MFe according to claim 52O4The preparation method of nanometer particle congery, it is characterised in that: described in step 1)
Macromolecule be polyvinylpyrrolidone, polyethyleneimine, polyacrylic acid or kayexalate.
7. MFe according to claim 62O4The preparation method of nanometer particle congery, it is characterised in that: institute in step 1)
The nanoparticle chloroformic solution concentration stated is 20 mg/mL.
8.MFe2O4Nanometer particle congery, it is prepared by method described in claim 1.
9. MFe described in claim 82O4Purposes of the nanometer particle congery in terms of light thermal property.
10. MFe described in claim 82O4Nanometer particle congery is answered photo-thermal therapy instrument, magnetic resonance imaging and bio-separation
With.
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| CN108192595A (en) * | 2018-01-25 | 2018-06-22 | 东北师范大学 | Magnetism-up-conversion nanoparticles aggregation and preparation method thereof |
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| CN108192595A (en) * | 2018-01-25 | 2018-06-22 | 东北师范大学 | Magnetism-up-conversion nanoparticles aggregation and preparation method thereof |
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