CN103772630B - A kind of preparation method of magnetic temperature sensing nano-particle - Google Patents
A kind of preparation method of magnetic temperature sensing nano-particle Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of magnetic temperature sensing nano-particle, it is the drawback existed for magnetic nano-particle, first silanization treatment is carried out to magnetic nano-particle, then graft polymerization is carried out, ultrasonic disperse, washing suction filtration, vacuum-drying, make magnetic temperature sensing nano-particle, this preparation method's technique is tight, rationally advanced, informative data is accurate, product morphology is good, for grey black powder granule, powder granule diameter≤220 nm, selected magnetic nano-particle has obvious superparamagnetism and there is one deck carbon coating layer on surface, can prevent from occurring between nanoparticle attracting each other causing coagulation in application process, the temperature sensitive effect of product is obvious, purity is high, reach 99%, production yield rate is high, reach 97.5%, it is the very good method preparing magnetic temperature sensing nano-particle, its product can at medicine, biotechnology and the application of multiple industrial circle.
Description
Technical field
The present invention relates to a kind of preparation method of magnetic temperature sensing nano-particle, belong to the technical field of the preparations and applicatio of magnetic field and temperature environment response nano particle.
Background technology
Environmental response nanoparticle is a kind of special functional nanoparticles, can to the specific stimulation from outside atmosphere, such as rapid reaction is made in temperature, potential of hydrogen, ionic strength, pressure, electric field, magnetic field, has stimulating responsive, is called intelligent nano particle; Because intelligent nano particle has unique physical chemistry and colloid property, there is great using value.
Magnetic temperature sensing nano-particle is a kind of nanoparticle possessing magnetic field and temperature effective, can be separated with medium quickly and easily under extraneous the action of a magnetic field, because temperature sensitive polymer has lowest critical solution temperature in aqueous, hydrogel can be formed after being water-swellable, when temperature is higher than lowest critical solution temperature, temperature sensitive polymer can shrink, water molecules in gel is discharged, with the wetting ability of this process nanoparticle, particle diameter, hole, electrophoresis and rheological property can change, this performance can make temperature sensitive polymer in drug release, bio-sensing, be applied in separation of biopolymer, therefore the magnetic temperature sensing nano-particle possessing magnetic field and temperature dual effect can be widely used in parting material and carrier, such as immunoassay, immobilized enzyme, target administration, the fields such as cellular segregation.
At present, the preparation of magnetic temperature sensing nano-particle is also in research, and also have a lot of not enough, such as step complexity is loaded down with trivial details, needs previously prepared magnetic nano-particle, is then combined with temperature sensitive polymer; At the temperature sensitive monomer of magnetic nano-particle surface grafting, easily cause attracting each other of magnetic nano-particle and produce coagulation; The size distribution of the magnetic temperature sensing nano-particle of preparation is wider, is unfavorable for application of process control, makes the application of magnetic temperature sensing nano-particle receive great limitation.
Summary of the invention
Goal of the invention
The object of the invention is the situation for background technology and deficiency, adopt at magnetic nano-particle modifying surface, the temperature sensitive monomer of graft polymerization, makes magnetic temperature sensing nano-particle, to improve the performance of magnetic temperature sensing nano-particle, expands use range.
Technical scheme
The chemical substance material used is: magnetic nano-particle, methacryloxypropyl trimethoxy silane, NIPA, N, N-methylene-bisacrylamide, Potassium Persulphate, dehydrated alcohol, deionized water, nitrogen, it is as follows that its combination prepares consumption: with gram, milliliter, centimetre
3for measure unit
Preparation method is as follows:
(1) silanization treatment magnetic nano-particle
Silanization treatment magnetic nano-particle stirs on ware carry out at there-necked flask, cleansing bath tub, ultrasonic disperse instrument, electric heating, completes under nitrogen protection, water cycle condensing state;
1. magnetic nano-particle 0.3g, methacryloxypropyl trimethoxy silane 1mL are added in there-necked flask;
Then by dehydrated alcohol 45mL, deionized water 15mL, be mixed with solution, add in there-necked flask;
2. there-necked flask is placed on ultrasonic disperse instrument, opens ultrasonic apparatus, ultrasonic disperse 20min under ultrasonic frequency 40kHz;
3., after ultrasonic disperse, there-necked flask is placed on cleansing bath tub;
4. water inlet pipe, the rising pipe of open water circulating condensing pipe, carry out water cycle condensation;
Open nitrogen valve, nitrogengas cylinder, to there-necked flask input nitrogen, nitrogen input speed 20cm
3/ min;
5. open electric heating and stir ware, temperature rises to 65 DEG C ± 2 DEG C, and starts to stir, and carries out Silanization reaction; Stirring, Silanization reaction time 120min, become magnetic nano-particle aaerosol solution;
Magnetic nano-particle will carry out chemical reaction in Silanization reaction process, and reaction formula is as follows:
In formula:
Fe
3o
4@C-C
9h
17o
5si: silanization magnetic nano-particle
CH
3oH: anhydrous methanol
6., after Silanization reaction, close electric heating and stir ware, make the silanization magnetic nano-particle aaerosol solution in there-necked flask be cooled to 25 DEG C with cleansing bath tub;
7. suction filtration
Silanization magnetic nano-particle aaerosol solution is placed in the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, remaining product filter cake on filter membrane, washings is evacuated in filter flask;
8. absolute ethanol washing, suction filtration
Product cake is placed in beaker, adds dehydrated alcohol 100mL, agitator treating 5min; Then washings is placed in the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, remaining product filter cake on filter membrane, washings is evacuated in filter flask;
Absolute ethanol washing, suction filtration repeat five times;
9. vacuum-drying
Product cake is placed in vacuum drying oven and carries out drying, drying temperature 40 DEG C, vacuum tightness 10Pa, time of drying, 480min, obtained after drying: silanization magnetic nano-particle
(2) silanization magnetic nano-particle surface grafting temperature sensitive polymer
Silanization magnetic nano-particle surface grafting temperature sensitive polymer stirs on ware carry out at four-hole boiling flask, cleansing bath tub, ultrasonic disperse instrument, electric heating, completes under nitrogen protection, water cycle condensing state;
1. prepare persulfate aqueous solution, take Potassium Persulphate 0.01g, measure deionized water 100mL, add in beaker, stir 30min, become the persulfate aqueous solution of 0.0037mol/L;
2. silanization magnetic nano-particle 0.1g, NIPA 0.5g and N,N methylene bis acrylamide 0.075g are added in there-necked flask; Add deionized water 25mL;
3. there-necked flask is placed on ultrasonic disperse instrument, opens ultrasonic apparatus, ultrasonic disperse 20min under ultrasonic frequency 40kHz;
4., after ultrasonic disperse, there-necked flask is placed on cleansing bath tub;
5. open water inlet pipe, the rising pipe of the water cycle prolong on there-necked flask, carry out water cycle condensation;
Open nitrogen valve, nitrogengas cylinder, to there-necked flask input nitrogen, nitrogen input speed 20cm
3/ min;
6. open electric heating and stir ware, temperature rises to 40 DEG C ± 2 DEG C, stirs 30min; Continue to be warming up to 70 DEG C ± 2 DEG C, add 0.0037mol/L persulfate aqueous solution 1mL, cause Raolical polymerizable; Stirring, polymerization reaction time 720min, become magnetic temperature sensing nano-particle aaerosol solution;
Silanization magnetic nano-particle will carry out chemical reaction in radical polymerization, and reaction formula is as follows:
In formula:
Fe
3o
4@C-C
22h
38o
8si: magnetic temperature sensing nano-particle
7., after Raolical polymerizable, close electric heating agitator, make the magnetic temperature sensing nano-particle aaerosol solution in there-necked flask be cooled to 25 DEG C with cleansing bath tub;
8. suction filtration
Magnetic temperature sensing nano-particle aaerosol solution is placed in the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, remaining product filter cake on filter membrane, washings is evacuated in filter flask;
9. absolute ethanol washing, suction filtration
Product cake is placed in beaker, adds dehydrated alcohol 100mL, agitator treating 5min; Then washings is placed in the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, remaining product filter cake on filter membrane, washings is evacuated in filter flask;
Absolute ethanol washing, suction filtration repeat five times;
10. vacuum-drying
Product cake is placed in vacuum drying oven and carries out drying, drying temperature 40 DEG C, vacuum tightness 10Pa, time of drying, 480min, obtained after drying: magnetic temperature sensing nano-particle;
(3) detect, analyze, characterize
The color and luster of magnetic temperature sensing nano-particle of preparation, pattern, structure, composition, chemical physics performance, absorbancy, concentration are detected, analyze, characterized;
Morphology analysis is carried out with transmission electron microscope;
Surface functional group analysis is carried out with infrared spectrometer;
Kinetic diameter analysis is carried out with dynamic optical diffractometer;
Conclusion: magnetic temperature sensing nano-particle is brownish black powder granule, particle diameter is≤220nm;
(4) product storage
Be stored in the Glass Containers of amber transparent to the magnetic temperature sensing nano-particle of preparation, airtightly keep in Dark Place, be placed in drying, clean environment, waterproof, sun-proof, moistureproof, anti-acid-alkali salt to corrode, storing temp 20 DEG C, relative humidity≤10%.
Beneficial effect
The present invention has obvious advance compared with background technology, first silanization treatment is carried out to magnetic nano-particle, then graft polymerization is carried out, through ultrasonic disperse, washing suction filtration, vacuum-drying, finally make magnetic temperature sensing nano-particle, this preparation method's technique is tight, rationally advanced, informative data is accurate, product morphology is good, for grey black powder granule, powder granule diameter≤220nm, selected magnetic nano-particle has obvious superparamagnetism and there is one deck carbon coating layer on surface, can prevent from occurring between nanoparticle attracting each other causing coagulation in application process, the temperature sensitive effect of product is obvious, purity is high, reach 99%, yield is high, reach 97.5%, it is the very good method preparing magnetic temperature sensing nano-particle, its product can at medicine, biotechnology and the application of multiple industrial circle.
Accompanying drawing explanation
Fig. 1 is magnetic temperature sensing nano-particle graft polymerization preparing processes figure
Fig. 2 is the transmission electron microscope shape appearance figure of magnetic nano-particle and magnetic temperature sensing nano-particle
Fig. 3 is NIPA, magnetic nano-particle and magnetic temperature sensing nano-particle infrared spectra comparison diagram
Fig. 4 is that magnetic temperature sensing nano-particle varies with temperature graphic representation at water medium power diameter
Shown in figure, list of numerals is as follows:
1, cleansing bath tub, 2, electric heating ware, 3, four-hole boiling flask, 4, nitrogen tube, 5, addition funnel, 6, control valve, 7, agitator, 8, water cycle prolong, 9, water shoot, 10, rising pipe, 11, air outlet, 12, anchor, 13, display screen, 14, pilot lamp, 15, power switch, 16, heating temperature control, 17, mixing control device, 18, nitrogengas cylinder, 19, nitrogen valve, 20, nitrogen, 21, water-bath water, 22, magnetic temperature sensing nano-particle aaerosol solution.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described further:
Shown in Fig. 1, be magnetic temperature sensing nano-particle graft polymerization preparing processes figure, each position, annexation want correct, and proportioning according to quantity, operates according to the order of sequence.
Magnetic temperature sensing nano-particle graft polymerization preparation is carried out in four-hole boiling flask, completes under water-bath, heating, stirring, water cycle condensation, nitrogen protection;
Cleansing bath tub 1 is rectangle, is electric heating ware 2 in the bottom of cleansing bath tub 1, places four-hole boiling flask 3, and fixed by anchor 12 on the top of cleansing bath tub 1; Nitrogen tube 4, addition funnel 5 and control valve 6, agitator 7, water cycle prolong 8 and water inlet pipe 9, rising pipe 10, air outlet 11 are set from left to right on four-hole boiling flask 3 top; Four-hole boiling flask inner bottom part is temperature sensitive magnetic nano-particle aaerosol solution 22; Nitrogen tube 4 connects nitrogengas cylinder 18 by nitrogen valve 19, and inputs nitrogen 20 in four-hole boiling flask 3; Be water-bath water 21 in cleansing bath tub 1, water-bath water 21 will flood 4/5 of four-hole boiling flask 3 volume; Electric heating ware 2 arranges display screen 13, pilot lamp 14, power switch 15, heating temperature control 16, mixing control device 17.
The value of the chemical substance that preparation uses determines according to the scope pre-set, with gram, milliliter, centimetre
3for measure unit.
Shown in Fig. 2, for the transmission electron microscope shape appearance figure of magnetic nano-particle a and magnetic temperature sensing nano-particle b, product is nucleocapsid structure, the outside coated carbon-coating of magnetic nano-particle, the carbon-coating periphery of magnetic temperature sensing nano-particle is coated with polymer layer, after the temperature sensitive monomer of grafting, the shell thickness of magnetic nano-particle increases to 38nm by original 30nm.
Shown in Fig. 3, be the infrared spectra comparison diagram of NIPA a, magnetic nano-particle b and magnetic temperature sensing nano-particle c, ordinate zou is transmitance, X-coordinate is wave number, in figure, known magnetic nano-particle is at 3433cm
-1the absorption peak at place illustrates that its surface is containing hydroxyl, and be conducive to silane coupling agent to be grafted to magnetic nano particle sub-surface, magnetic temperature sensing nano-particle possesses the absorption peak of raw material magnetic nano-particle and NIPA simultaneously: 3433cm
-1the stretching vibration peak of the O-H that place's magnetic nano particle sub-surface does not react completely, 2966cm
-1and 2925cm
-1place is-CH
2-and-CH
3-C-H-stretching vibration peak, 1628cm
-1place is the stretching vibration peak of C=O, 1120cm
-1place is-C (CH
3) C-C skeleton stretching vibration peak.
Shown in Fig. 4, for magnetic temperature sensing nano-particle varies with temperature graphic representation at water medium power diameter, ordinate zou is kinetic diameter, and X-coordinate is temperature, and in figure, the kinetic diameter of known magnetic temperature sensing nano-particle is along with the increase of temperature, start to remain unchanged, then sharply decline, finally constant, obvious about 45 DEG C downtrendings, illustrate that this particle has significant temperature sensitive effect, and Volume-phase transition temperature is 45 DEG C.
Claims (2)
1. the preparation method of a magnetic temperature sensing nano-particle, it is characterized in that: the chemical substance material of use is: magnetic nano-particle, methacryloxypropyl trimethoxy silane, NIPA, N, N-methylene-bisacrylamide, Potassium Persulphate, dehydrated alcohol, deionized water, nitrogen, it is as follows that its combination prepares consumption: with gram, milliliter, centimetre
3for measure unit
Preparation method is as follows:
(1) silanization treatment magnetic nano-particle
Silanization treatment magnetic nano-particle stirs on ware carry out at there-necked flask, cleansing bath tub, ultrasonic disperse instrument, electric heating, completes under nitrogen protection, water cycle condensing state;
1. magnetic nano-particle 0.3g, methacryloxypropyl trimethoxy silane 1mL are added in there-necked flask;
Then by dehydrated alcohol 45mL, deionized water 15mL, be mixed with solution, add in there-necked flask;
2. there-necked flask is placed on ultrasonic disperse instrument, opens ultrasonic apparatus, ultrasonic disperse 20min under ultrasonic frequency 40kHz;
3., after ultrasonic disperse, there-necked flask is placed on cleansing bath tub;
4. water inlet pipe, the rising pipe of open water circulating condensing pipe, carry out water cycle condensation;
Open nitrogen valve, nitrogengas cylinder, to there-necked flask input nitrogen, nitrogen input speed 20cm
3/ min;
5. open electric heating and stir ware, temperature rises to 65 DEG C ± 2 DEG C, and starts to stir, and carries out Silanization reaction; Stirring, Silanization reaction time 120min, become magnetic nano-particle aaerosol solution;
Magnetic nano-particle will carry out chemical reaction in Silanization reaction process, and reaction formula is as follows:
In formula:
Fe
3o
4@C-C
9h
17o
5si: silanization magnetic nano-particle
CH
3oH: anhydrous methanol
6., after Silanization reaction, close electric heating and stir ware, make the silanization magnetic nano-particle aaerosol solution in there-necked flask be cooled to 25 DEG C with cleansing bath tub;
7. suction filtration
Silanization magnetic nano-particle aaerosol solution is placed in the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, remaining product filter cake on filter membrane, washings is evacuated in filter flask;
8. absolute ethanol washing, suction filtration
Product cake is placed in beaker, adds dehydrated alcohol 100mL, agitator treating 5min; Then washings is placed in the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, remaining product filter cake on filter membrane, washings is evacuated in filter flask;
Absolute ethanol washing, suction filtration repeat five times;
9. vacuum-drying
Product cake is placed in vacuum drying oven and carries out drying, drying temperature 40 DEG C, vacuum tightness 10Pa, time of drying, 480min, obtained after drying: silanization magnetic nano-particle
(2) silanization magnetic nano-particle surface grafting temperature sensitive polymer
Silanization magnetic nano-particle surface grafting temperature sensitive polymer stirs on ware carry out at four-hole boiling flask, cleansing bath tub, ultrasonic disperse instrument, electric heating, completes under nitrogen protection, water cycle condensing state;
1. prepare persulfate aqueous solution, take Potassium Persulphate 0.01g, measure deionized water 100mL, add in beaker, stir 30min, become the persulfate aqueous solution of 0.0037mol/L;
2. silanization magnetic nano-particle 0.1g, NIPA 0.5g and N,N methylene bis acrylamide 0.075g are added in there-necked flask; Add deionized water 25mL;
3. there-necked flask is placed on ultrasonic disperse instrument, opens ultrasonic apparatus, ultrasonic disperse 20min under ultrasonic frequency 40kHz;
4., after ultrasonic disperse, there-necked flask is placed on cleansing bath tub;
5. open water inlet pipe, the rising pipe of the water cycle prolong on there-necked flask, carry out water cycle condensation;
Open nitrogen valve, nitrogengas cylinder, to there-necked flask input nitrogen, nitrogen input speed 20cm
3/ min;
6. open electric heating and stir ware, temperature rises to 40 DEG C ± 2 DEG C, stirs 30min; Continue to be warming up to 70 DEG C ± 2 DEG C, add 0.0037mol/L persulfate aqueous solution 1mL, cause Raolical polymerizable; Stirring, polymerization reaction time 720min, become magnetic temperature sensing nano-particle aaerosol solution;
Silanization magnetic nano-particle will carry out chemical reaction in radical polymerization, and reaction formula is as follows:
In formula:
Fe
3o
4@C-C
22h
38o
8si: magnetic temperature sensing nano-particle
7., after Raolical polymerizable, close electric heating agitator, make the magnetic temperature sensing nano-particle aaerosol solution in there-necked flask be cooled to 25 DEG C with cleansing bath tub;
8. suction filtration
Magnetic temperature sensing nano-particle aaerosol solution is placed in the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, remaining product filter cake on filter membrane, washings is evacuated in filter flask;
9. absolute ethanol washing, suction filtration
Product cake is placed in beaker, adds dehydrated alcohol 100mL, agitator treating 5min; Then washings is placed in the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, remaining product filter cake on filter membrane, washings is evacuated in filter flask;
Absolute ethanol washing, suction filtration repeat five times;
10. vacuum-drying
Product cake is placed in vacuum drying oven and carries out drying, drying temperature 40 DEG C, vacuum tightness 10Pa, time of drying, 480min, obtained after drying: magnetic temperature sensing nano-particle;
(3) detect, analyze, characterize
The color and luster of magnetic temperature sensing nano-particle of preparation, pattern, structure, composition, chemical physics performance, absorbancy, concentration are detected, analyze, characterized;
Morphology analysis is carried out with transmission electron microscope;
Surface functional group analysis is carried out with infrared spectrometer;
Kinetic diameter analysis is carried out with dynamic optical diffractometer;
Conclusion: magnetic temperature sensing nano-particle is brownish black powder granule, particle diameter is≤220nm;
(4) product storage
Be stored in the Glass Containers of amber transparent to the magnetic temperature sensing nano-particle of preparation, airtightly keep in Dark Place, be placed in drying, clean environment, waterproof, sun-proof, moistureproof, anti-acid-alkali salt to corrode, storing temp 20 DEG C, relative humidity≤10%.
2. the preparation method of a kind of magnetic temperature sensing nano-particle according to claim 1, it is characterized in that: described magnetic temperature sensing nano-particle graft polymerization preparation is carried out in four-hole boiling flask, completes under water-bath, heating, stirring, water cycle condensation, nitrogen protection;
Cleansing bath tub (1) is rectangle, is electric heating ware (2), puts four-hole boiling flask (3) on the top of cleansing bath tub (1) in the bottom of cleansing bath tub (1), and is fixed by anchor (12); Nitrogen tube (4), addition funnel (5) and control valve (6), agitator (7), water cycle prolong (8) and water inlet pipe (9), rising pipe (10), air outlet (11) are set from left to right on four-hole boiling flask (3) top; Four-hole boiling flask inner bottom part is temperature sensitive magnetic nano-particle aaerosol solution (22); Nitrogen tube (4) connects nitrogengas cylinder (18) by nitrogen valve (19), and input nitrogen (20) in four-hole boiling flask (3); Be water-bath water (21) in cleansing bath tub (1), water-bath water (21) to flood and four-hole boiling flask (3) volume 4/5; Electric heating ware (2) arranges display screen (13), pilot lamp (14), power switch (15), heating temperature control (16), mixing control device (17).
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| CN107115528A (en) * | 2017-05-26 | 2017-09-01 | 山西医科大学第二医院 | A kind of preparation method with the order mesoporous Nano carbon balls of the temperature sensitive magnetic of temperature controlled release and magnetic heat-therapeutic action |
| CN107441498A (en) * | 2017-06-12 | 2017-12-08 | 安徽省颍上县正泰电器有限责任公司 | A kind of preparation method of the carbon nano-tube modified composite stone wax powder powder material of nano-cellulose |
| CN112538145A (en) * | 2020-12-23 | 2021-03-23 | 西南石油大学 | Preparation method and application of intelligent controlled-release targeting nano oil-displacing agent microcapsule |
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| CN1995144A (en) * | 2006-12-22 | 2007-07-11 | 淮阴师范学院 | Method for synthesizing magnetic temperature-sensitive nano particle |
| CN100575376C (en) * | 2007-10-26 | 2009-12-30 | 中山大学 | A kind of magnetic temperature sensing nano-particle and synthetic method thereof with biocompatibility |
| CN102417567B (en) * | 2011-11-17 | 2013-05-08 | 西北工业大学 | Preparation method for one-dimensional magnetic thermo-sensitivity nanochain |
| CN103319657A (en) * | 2013-07-15 | 2013-09-25 | 天津工业大学 | Thermo-sensitive type magnetic levosulpiride molecularly-imprinted microsphere and preparation method thereof |
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