CN110373030A - A kind of induced by magnetic field patterning assembling and erasable magnetic control phase-change material and preparation method thereof - Google Patents
A kind of induced by magnetic field patterning assembling and erasable magnetic control phase-change material and preparation method thereof Download PDFInfo
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- 238000000059 patterning Methods 0.000 title claims abstract description 32
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- 239000002086 nanomaterial Substances 0.000 claims abstract description 70
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- 239000006249 magnetic particle Substances 0.000 description 4
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910001172 neodymium magnet Inorganic materials 0.000 description 1
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- 125000001273 sulfonato group Chemical group [O-]S(*)(=O)=O 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/0018—Diamagnetic or paramagnetic materials, i.e. materials with low susceptibility and no hysteresis
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The present invention discloses a kind of induced by magnetic field patterning assembling and erasable magnetic control phase-change material and preparation method thereof.The magnetic control phase-change material is using polarity or nonpolar low temperature phase change high molecular material as basis material, and using surface polarity or the modified superparamagnetic nanomaterial of nonpolarity as magnetic responsiveness unit, the mass ratio of magnetic responsiveness unit and basis material is 0.2~0.5:1；Wherein, basis material is identical as the molecular polarity of magnetic responsiveness unit.By modified to Superparamagnetic particulates surface, it is made to possess the surface nature for being dissolved in corresponding phase-change material, then with effectively stable compound of phase transformation matrix, is uniformly dispersed and can get the magnetic control phase-change material having to magnetic field quick response；The material passes through magnetic field array at high temperature and completes patterning assembling, when temperature is reduced to fusing point or less, which has shape stability at no magnetic field, when temperature increases again to more than fusing point, without under magnetic fields, which can realize the erasing of pattern by Self-leveling.
Description
Technical field
The present invention relates to a kind of magnetic control phase-change material, in particular to a kind of induced by magnetic field patterning assembling and erasable magnetic
Phase-change material and preparation method thereof is controlled, belongs to picture on surface and constructs and surface-functionalized application field.
Background technique
Functionalizing material surface and patterning techniques are constantly subjected to the close attention of people.Conventional surface technology of preparing is main
There are printing, spraying, engraving and pressing mold.These technologies have extremely wide in wide area surface processing and templating surface manufacture field
General application.The surface preparation technology of modernization has chemical etching method, self-assembly method and photoetching process etc..These technologies can be fine
The defect for making up traditional technology and being included, have very huge work for the surface modification of present information material and energy and material
With.From traditional technology to modern technologies, the surface of many method preparations is all permanent, it is difficult to it wipes and constructs again, and
And picture on surface to construct the time longer.
In recent years, it is emerged one after another using the method that electric field, magnetic field are surface-treated.It the use of most wide method is to utilize band
Charged particle or magnetic particle carry out self assembly in electric field or magnetic field environment, to construct picture on surface.These particle surface bands
Active functional group to form firm combination with surface, and usually can quickly form pattern (such as Shen under environmental induction on the scene
Number self assembly kreatinin molecular imprinting film under induced by magnetic field please be disclosed for a Chinese invention patent application of 201310297744.X
Method, and electrochemical sensor is prepared with this；Application No. is CN201811135321.7 Chinese invention patent applications to disclose
A kind of method for inducing auxiliary electrojet to carry out fine 3D printing using electric field).
But these patterns once being formed after also can not just wipe.Although in addition, can be in magnetic field using conventional magnetic fluid
Patterning assembling is carried out under induction, but loses shape stability immediately after removing magnetic field.
Therefore, patterning assembling can be carried out and can stablize after removing magnetic field to deposit under induced by magnetic field by needing one kind
, while the material that can be wiped again if necessary.
Summary of the invention
Goal of the invention: it cannot keep pattern form for the patterning assembling of existing induced by magnetic field and be stabilized and pattern shape
The problem of can not wiping after, the application provide a kind of induced by magnetic field patterning assembling and erasable magnetic control phase-change material, together
When, the present invention also provides a kind of preparation methods of magnetic control phase-change material.
Technical solution: the assembling of induced by magnetic field of the present invention patterning and erasable magnetic control phase-change material, for based on
Magnetic-particle is melted into the magnetic control phase-change material that low-temperature phase-change material is combined, with polarity or nonpolar low temperature phase change macromolecule
Material is basis material, using the modified superparamagnetic nanomaterial of surface polarity or nonpolarity as magnetic responsiveness unit, wherein magnetic
The mass ratio of field response unit and basis material is 0.2~0.5:1.
In magnetic control phase-change material, basis material is identical as the molecular polarity of magnetic responsiveness unit, i.e. the magnetic control phase-change material
Composition can be divided into two kinds:
The first is compound for the modified superparamagnetic nanomaterial of surface polarity and polarity low temperature phase change high molecular material
Material, wherein the modified superparamagnetic nanomaterial of surface polarity is that the high molecular superparamagnetism of surface grafting polar long chain is received
Rice material, polarity low temperature phase change macromolecule can be polyethylene glycol, poly glycol monomethyl ether, polyethylene glycol dimethyl ether, double-end amino
The hydrophilies low temperature phase change macromolecule such as polyethylene glycol or Carboxylic-terminated Polyethylene Glycol.
Second is the modified superparamagnetic nanomaterial of surface nonpolarity and nonpolar low temperature phase change high molecular material
Composite material: where nonpolarity modified superparamagnetic nanomaterial in surface is the super of surface grafting nonpolarity long chain macromolecule
Paramagnetic nanoparticles material, nonpolar low temperature phase change macromolecule can be the hydrophobicitys low temperature such as long-chain fat alkane at different levels and its modified body
Phase transformation macromolecule, such as solid paraffin, docosane, octadecane, octadecylamine, two tetradecy lamines, octadecyl alcolol etc.；It is preferably selected stone
Wax.
In above two magnetic control phase-change material, superparamagnetic nanomaterial is selected from nanometer iron powder, nano ferriferrous oxide, receives
Rice iron oxide, nano-nickel powder, nano-cobalt powder etc., preferably nano ferriferrous oxide.
The preparation method of induced by magnetic field patterning assembling and erasable magnetic control phase-change material of the present invention, including such as
Lower step:
(1) superparamagnetic nanomaterial that surface polarity or nonpolarity are modified is prepared；
(2) corresponding polarity or nonpolar low temperature is added in the modified superparamagnetic nanomaterial of surface polarity or nonpolarity
In phase transformation macromolecule, grinding, make magnetic responsiveness unit in basis material it is evenly dispersed to get.
In the first magnetic control phase-change material, the modified superparamagnetic nanomaterial of surface polarity the preparation method comprises the following steps: to super
Paramagnetic nanoparticles material surface is pre-processed, and introduces quaternary ammonium salt ionic group on its surface；Then by polar long chain macromolecule
Anion salt is grafted to pretreatment gained particle surface, obtains the modified superparamagnetic nanomaterial of surface polarity.The preparation side
Method specifically may include following step:
1. superparamagnetic nanomaterial is added to the water, with dimethyl stearyl [3- trimethoxy silicon propyl] ammonium chloride
For modifying agent, ageing reaction 12~24 hours at room temperature, or reacted 1~3 hour at 60~80 DEG C, products therefrom water and
Methanol is repeatedly washed, is separated, and obtains the superparamagnetic nanomaterial that surface introduces quaternary ammonium salt ionic group；
In this step, being aged the reaction time at room temperature is preferably 24 hours；It can accelerate reaction by heating mode to carry out, such as
It need to only be reacted 1~3 hour at 60~80 DEG C, optimum reaction condition is to react 2 hours at 75 DEG C.
2. polyethylene glycol groups macromolecule sulfonic acid salt is held at 65~80 DEG C with pretreated superparamagnetic nanomaterial
Continuous reaction 12~24 hours, the mixed solution of product water and methanol after reaction washs, and removes surface unmodified in product
The superparamagnetic nanomaterial superparamagnetic nanomaterial modified to get surface polarity.The process of grafting of this step is best
Reaction condition is to react 24 hours at 75 DEG C.
Wherein, polyethylene glycol groups macromolecule sulfonic acid salt is by polyethylene glycol groups high molecular material by sulfonation processing, by its end
Hydroxy functional group reaction is obtained at end sulfonate functional；Polyethylene glycol groups high molecular material is selected from poly glycol monomethyl ether, gathers
Ethylene glycol list oil ether, fatty alcohol polyoxyethylene ether etc., and the molecular weight ranges of polyethylene glycol groups high molecular material be 500~
4000.Preferably, polyethylene glycol groups macromolecule sulfonic acid salt the preparation method comprises the following steps: to different molecular weight polyethylene glycol based high molecular
Sulfamic acid and urea are added in material, is heated to 120 DEG C and reacts 4~5 hours, dissolved after the reaction was completed with a large amount of ethyl alcohol, mistake
Filter, volatilize to get.
In second of magnetic control phase-change material, the modified superparamagnetic nanomaterial of surface nonpolarity the preparation method comprises the following steps: right
Superparamagnetic nanomaterial surface is pre-processed, and introduces epoxy group on its surface；Then nonpolarity Amino End Group modified
Long-chain is grafted to pretreatment gained particle surface, obtains the modified superparamagnetic nanomaterial of surface nonpolarity.The preparation method
May include specifically following step:
1. superparamagnetic nanomaterial is added in ethanol solution, with γ-glycidyl ether oxygen propyl trimethoxy silicane
It for modifying agent, is reacted at 65~80 DEG C 2~3 hours, uses ethanol washing, drying after reaction, obtained surface and introduce epoxy
The superparamagnetic nanomaterial of group；The optimum reaction condition of this step is to react 2 hours at 70 DEG C；
2. the product after drying is added in n,N-Dimethylformamide, long chain alkane amine is added, it is anti-at 60~80 DEG C
It answers 3~5 hours, Magneto separate, is washed with carbon tetrachloride solution after reaction, removes superparamagnetism surface unmodified in product
The nano material superparamagnetic nanomaterial modified to get surface nonpolarity.The optimum reaction condition of this step is anti-at 65 DEG C
It answers 4 hours.
After surface polarity or nonpolar superparamagnetic nanomaterial is made, preferably polarity or nonpolar low-temperature phase are got higher
Molecule is first to heat to 10 DEG C higher than its fusing point or more of temperature, and the superparamagnetism that surface polarity or nonpolarity are modified then is added and receives
Rice material；Preferably, the additional amount for the superparamagnetic nanomaterial that surface polarity or nonpolarity are modified is that polarity or nonpolarity are low
The 20~50% of warm phase transformation high molecule mass；Preferably the 30% of polarity or nonpolar low temperature phase change high molecule mass.
The method of induced by magnetic field patterning assembling is carried out using the magnetic control phase-change material of the application and method for deleting is respectively as follows:
(1) induced by magnetic field patterns packaging technology
Using permanent magnet cylindrical body as pixel, different pattern is constructed using array mould plate, using non magnetic heating plate
Load plane as magnetic control phase-change material: heating plate is placed in above permanent magnet array, temperature is increased to magnetic control phase transformation material
More than the fusing point of material, under magnetic fields, the magnetic control phase-change material of thawing is to permanent magnet array surface enrichment；Temperature is reduced to
The pattern constructed is carried out shaping below magnetic control phase-change material fusing point.
Permanent magnet material can be ndfeb magnet cylindrical body, and diameter is generally 2~100mm, magnetic field strength is 200~
500mT；Array template can be prepared by way of casting, injection molding or 3D printing；Non magnetic heating plate is by glass or plastic plate
Deng composition.
(2) erasing technique
When needing to wipe, the heating plate with magnetic control phase change material pattern is removed from permanent magnet array, by temperature liter
More than height to magnetic control phase-change material fusing point, phase-change material realizes the auto-erasing of pattern by Self-leveling.
The utility model has the advantages that compared with prior art, advantages of the present invention are as follows: (1) magnetic control phase-change material of the invention can be
It is realized when temperature is increased to fusing point or more by patterned induced by magnetic field and is enriched in the patterning of different surfaces, and pass through crystallization
It realizes and stablizes without the pattern under magnetic field, it can also be under no magnetic fields, by the way that temperature is increased to fusing point implementation above pattern
Self-leveling erasing；(2) present invention is mutually got higher it with Different hypothermia by being modified to super suitable superparamagnetic nanomaterial
Molecular material carries out compound, and be prepared two kinds of different substrates of polarity and nonpolarity can induced by magnetic field patterning assembling and can
The polymer composite of erasing, method is easy, lower cost for material；Moreover, easily passing through control phase transformation high molecular material molecule
Amount is to adjust material phase transformation temperature, liquid fluidity and solid-state mechanical property.
Detailed description of the invention
Fig. 1 is the TEM figure and infared spectrum of the modified superparamagnetic nanomaterial of surface nonpolarity made from embodiment 1；
Fig. 2 is the TEM figure and infared spectrum of the modified superparamagnetic nanomaterial of surface polarity made from embodiment 2；
Fig. 3 is the change in physical figure in the reversible erase process of magnetic control phase-change material prepared by embodiment 1；
Fig. 4 is the structural schematic diagram of the permanent magnet magnetism array mould plate prepared when induced by magnetic field patterning assembling experiment；
Fig. 5 be under induced by magnetic field, using magnetic control phase-change material made from embodiment 1 Fig. 4 permanent magnet array template
On obtained response pattern.
Specific embodiment
Technical solution of the present invention is described further with reference to the accompanying drawing.
A kind of induced by magnetic field patterning assembling of the invention and erasable magnetic control phase-change material, to be melted based on magnetic-particle
Its surface is modified, is made using existing Superparamagnetic particulates in the magnetic control phase-change material that low-temperature phase-change material is combined
It possesses the surface nature for being melted into corresponding phase-change material, then by modified magnetic particle with phase transformation matrix is effectively stable answers
It closes, is uniformly dispersed and can get the phase-change material having to magnetic field quick response.
The magnetic control phase-change material is composite material, using polarity or nonpolar low temperature phase change high molecular material as matrix material
Material, using the modified superparamagnetic nanomaterial of surface polarity or nonpolarity as magnetic responsiveness unit, wherein magnetic responsiveness unit and
The mass ratio of basis material is 0.2~0.5:1.In magnetic control phase-change material, the molecular polarity of basis material and magnetic responsiveness unit
Identical, i.e., the composition of the magnetic control phase-change material can be divided into two kinds: the first is the modified superparamagnetic nanomaterial of surface polarity
With the composite material of polarity low temperature phase change high molecular material, second for the modified superparamagnetic nanomaterial of surface nonpolarity and
The composite material of nonpolar low temperature phase change high molecular material.
Wherein, the modified superparamagnetic nanomaterial of surface polarity is the high molecular superparamagnetism of surface grafting polar long chain
Nano material, the modified superparamagnetic nanomaterial of surface nonpolarity are the superparamagnetism of surface grafting nonpolarity long chain macromolecule
Nano material, superparamagnetic nanomaterial are selected from nanometer iron powder, nano ferriferrous oxide, nano iron oxide, nano-nickel powder, nanometer
Cobalt powder etc..Polarity low temperature phase change macromolecule can be polyethylene glycol, poly glycol monomethyl ether, polyethylene glycol dimethyl ether, double-end amino
The hydrophilies low temperature phase change macromolecule such as polyethylene glycol or Carboxylic-terminated Polyethylene Glycol；Nonpolar low temperature phase change macromolecule can be at different levels
The hydrophobicitys low temperature phase change macromolecule such as long-chain fat alkane and its modified body, such as solid paraffin, docosane, octadecane, ten
Eight amine, two tetradecy lamines, octadecyl alcolol etc..
Embodiment 1
Modified superparamagnetic nanomaterial/low temperature phase change non-polar high polymer composite material the preparation of surface nonpolarity
(1) 0.5g nanometer Fe is weighed3O4It is added in the anhydrous n,N-Dimethylformamide of 80mL (DMF), ultrasonic half an hour,
Ensure stable dispersion, it is molten that the ethyl alcohol that 1mL contains 20% γ-glycidyl ether oxygen propyl trimethoxy silicane surfactant is added dropwise
Liquid, solution are added in three-necked flask, and ethanol washing, drying are used in mechanic whirl-nett reaction 2 hours at 70 DEG C after reaction；
(2) product after drying is added in 100mL DMF, 0.8g octadecylamine is added, is reacted 5 hours at 80 DEG C,
After Magneto separate, washed with DMF hot solution, remaining octadecylamine of going out, with carbon tetrachloride dissolve superparamagnetic nanomaterial,
Insoluble body is removed by filtering, solution is volatilized to obtain the superparamagnetic nanomaterial being modified, TEM figure and infared spectrum are such as
Fig. 1；
(3) superparamagnetic nanomaterial containing octadecylamine long-chain prepared is incorporated into paraffin phase, it is long containing octadecylamine
The quality of the superparamagnetic nanomaterial of chain is 0.5g, Quality of Paraffin Waxes 2.5g, ensures superparamagnetic nanomaterial by grinding
It is evenly dispersed in paraffin matrix, it is prepared into paraffinic base magnetic control phase-change material.
Reversible erasing experiment and induced by magnetic field patterning are carried out using paraffinic base magnetic control phase-change material manufactured in the present embodiment
Assembling experiment:
Test a reversible erasing experiment
Fig. 3 is that magnetic control phase-change material is successively patterned from reset condition, pattern is stable made from embodiment 1, pattern is wiped
Except the liquid solid state Transformation Graphs in whole process, wherein (a) figure is the magnetic control phase-change material in planar solid form, the shape
Magnetic response manipulation can not be carried out under state；(b) figure is the magnetic control phase-change material in flat liquid form, it is by consolidating in (a) figure
State plane is by being thermally formed, and surface is in flowable state at this time, has magnetic response property；(c) the liquid phase magnetic control phase transformation material in figure
Material converges to magnetic field most strength by the permanent magnet driving under loading plate, is in steamed bun peak form, remains liquid phase after convergence；
(d) figure is formed by the material cooled and solidified in (c) figure, and magnetic control phase-change material maintains the shape of (c) figure at this time, but its phase
State is converted into solid-state, can not carry out magnetic control manipulation again at this time, shape remains unchanged after removing magnetic field；(e) figure is (d) figure steamed bun peak
Picture after thawing, material erases shape by Self-leveling, reverts to flat liquid shape again at liquid after heat temperature raising
State can carry out next step magnetic control write-in.This five figures illustrate the reversible erasable complete procedure in magnetic control surface.
Test the patterning assembling experiment of two induced by magnetic field
Determine needed for magnetic array display precision be 15 multiplied by 15 array, pass through 3dmax modeling software construct magnetic control
Array template prototype, template is having a size of 16cm multiplied by 16cm, and with a thickness of 1.5cm, jack diameter is 4.2mm, and jack spacing is
8mm, jack depth are 6mm, implement the construction of entity by 3D printing, finally print obtained permanent magnet array template such as Fig. 4,
Its array point can be analogous to pixel, and the arrangement by being inserted into permanent magnet can effectively control change in pattern.
The Nd-Fe-B permanent magnet of purchase having a size of diameter be 4mm, length 12mm, as field generating unit, always
Number is 225, is inserted into corresponding template gap according to pattern requirement, constructs the battle array of the three-dimensional magnetic field based on plane pattern with this
Column are prepared into three-dimensional material array when magnetic fluid once nearby accumulation will be attracted by magnetic field array element.Magnetic control
Manipulation technology is then to do linear combination as traction device using two permanent magnets to be mounted in the electrical mobile device of plane, in electricity
Manipulation lower traction magnetic fluid in brain end regulates and controls magnetic strength by the distance between magnet and fluid plate to designated position.
Fig. 5 is that induced by magnetic field patterning assembling gained magnetic control picture on surface is carried out under permanent magnet array template shown in Fig. 4,
Pattern structure is accurate, and the central point at each peak is overlapped with template permanent magnet center, illustrates the magnetic control phase-change material in magnetic field array
Picture on surface can be rapidly constructed under effect.
Embodiment 2
Modified superparamagnetic nanomaterial/low temperature phase change polarity polymer composite the preparation of surface polarity
(1) 0.5g nanometer Fe is weighed3O4It is added in 10mL water, 3mL dimethyl stearyl [3- trimethoxy silicon is added
Propyl] ammonium chloride methanol solution (mass fraction 40%), the ammonia spirit of pH=12 is added dropwise, adjusting pH is 10, is stirred at room temperature
Ageing 24 hours, is repeatedly washed with water and methanol, and Magneto separate is dissolved with tetrahydrofuran, is filtered and is removed insoluble body, solution is waved
The dry superparamagnetic nanomaterial for containing quaternary ammonium salt functional to get surface；
(2) it weighs and 0.5g sulfamic acid and 0.08g urea is added in the poly glycol monomethyl ether that 10g molecular weight is 2000,
It is heated to 120 DEG C to react 5 hours, be dissolved after the reaction was completed with 100mL ethyl alcohol, filtering volatilizes, obtains having sulfonate end group
Polysalt；
(3) 0.5g quaternary ammonium salt superparamagnetic nanomaterial and 10mL poly glycol monomethyl ether sulfonic acid saline solution (matter are weighed
Amount score is 20%) to stir 24 hours at 75 DEG C, and product Magneto separate is washed with toluene, is filtered, and insoluble body is removed, final to obtain
To the superparamagnetic nanomaterial modified containing overlength polyethylene glycol segment, TEM figure and infared spectrum such as Fig. 2；
(4) weigh 1g contain overlength polyethylene glycol segment modification superparamagnetic nanomaterial be added to quality be 2g, point
Son amount is in 4000 polyethylene glycol matrix, polyethylene glycol groups magnetic control phase-change material is prepared in grinding distribution.
Referring to the method in embodiment 1, magnetic field is carried out using polyethylene glycol groups magnetic control phase-change material made from the present embodiment
Induced patterning assembling experiment and reversible erasing experiment, the results showed that, polarity polyethylene glycol groups magnetic control phase made from the present embodiment
Becoming material also can be realized induced by magnetic field patterning assembling, and pattern can be stablized and can reversible erasing under no magnetic field.
Embodiment 3
Modified superparamagnetic nanomaterial/low temperature phase change the non-polar high polymer of surface nonpolarity is prepared referring to embodiment 1
Composite material, difference are, in step (2), the reaction temperature of nano magnetic material and alkane amine with epoxy group is 65
DEG C, the reaction time is 4 hours.
Embodiment 4
Modified superparamagnetic nanomaterial/low temperature phase change polarity the high score of surface polarity is prepared referring to the method for embodiment 2
Sub- composite material, difference are: in step (1), accelerating ageing reaction by heating and carry out: by 0.5g nanometer Fe3O480mL is added
In water, temperature rises to 75 DEG C, and dimethyl stearyl [3- trimethoxy silicon propyl] ammonium chloride of 3mL mass fraction 40% is added
The ammonia spirit of pH=12 is added dropwise in methanol solution, adjusts the pH to 10 of solution, is stirred to react 2 hours.
Claims (10)
1. a kind of induced by magnetic field patterning assembling and erasable magnetic control phase-change material, which is characterized in that the magnetic control phase-change material
Using polarity or nonpolar low temperature phase change high molecular material as basis material, received with the superparamagnetism that surface polarity or nonpolarity are modified
Rice material is magnetic responsiveness unit, and the mass ratio of magnetic responsiveness unit and basis material is 0.2~0.5:1；The magnetic control phase
Become in material, basis material is identical as the molecular polarity of magnetic responsiveness unit.
2. induced by magnetic field patterning assembling according to claim 1 and erasable magnetic control phase-change material, which is characterized in that
The superparamagnetic nanomaterial that the surface polarity or nonpolarity are modified is surface grafting polarity or nonpolar long chain macromolecule
Superparamagnetic nanomaterial, wherein the superparamagnetic nanomaterial is nanometer iron powder, nano ferriferrous oxide, nano oxidized
One or more of iron, nano-nickel powder, nano-cobalt powder.
3. induced by magnetic field patterning assembling according to claim 1 and erasable magnetic control phase-change material, which is characterized in that
The polarity low temperature phase change high molecular material is hydrophily low temperature phase change macromolecule, which is poly- second
Glycol, poly glycol monomethyl ether, polyethylene glycol dimethyl ether, amino-end peg or Carboxylic-terminated Polyethylene Glycol；It is described non-
Polarity low temperature phase change high molecular material is hydrophobicity low temperature phase change macromolecule, which is selected from length at different levels
Chain fatty alkane and its modified body.
4. a kind of preparation method of induced by magnetic field patterning assembling and erasable magnetic control phase-change material described in claim 1,
It is characterized by comprising the following steps:
(1) superparamagnetic nanomaterial that surface polarity or nonpolarity are modified is prepared；
(2) corresponding polarity or nonpolar low temperature phase change is added in the modified superparamagnetic nanomaterial of surface polarity or nonpolarity
In high molecular material, grinding, make magnetic responsiveness unit in basis material it is evenly dispersed to get.
5. the preparation method of induced by magnetic field patterning assembling and erasable magnetic control phase-change material according to claim 4,
It is characterized in that, in step (1), the modified superparamagnetic nanomaterial of the surface polarity the preparation method comprises the following steps: to superparamagnetic
Property nano-material surface pre-processed, its surface introduce quaternary ammonium salt ionic group；Then by polar long chain macromolecule yin from
Alite is grafted to pretreatment gained particle surface, obtains the modified superparamagnetic nanomaterial of surface polarity.
6. the preparation method of induced by magnetic field patterning assembling and erasable magnetic control phase-change material according to claim 5,
It is characterized in that, the preparation step for the superparamagnetic nanomaterial that the surface polarity is modified includes:
It is to change with dimethyl stearyl [3- trimethoxy silicon propyl] ammonium chloride 1. superparamagnetic nanomaterial is added to the water
Property agent, ageing reaction 12~24 hours at room temperature, or reacted 1~3 hour at 60~80 DEG C, products therefrom water and methanol
Repeatedly washing, separation obtain the superparamagnetic nanomaterial that surface introduces quaternary ammonium salt ionic group；
2. polyethylene glycol groups macromolecule sulfonic acid salt and pretreated superparamagnetic nanomaterial are continued instead at 65~80 DEG C
It answers 12~24 hours, the mixed solution of product water and methanol after reaction washs, and removes surface unmodified super suitable in product
Magnetic Nano material to get.
7. the preparation method of induced by magnetic field patterning assembling and erasable magnetic control phase-change material according to claim 6,
It is characterized in that, step 2. in, the polyethylene glycol groups macromolecule sulfonic acid salt passes through sulfonation by polyethylene glycol groups high molecular material
Processing obtains, wherein polyethylene glycol groups high molecular material is selected from poly glycol monomethyl ether, polyethyleneglycol oil ether, poly alkyl alcohol
Ethylene oxide ether, and the molecular weight ranges of polyethylene glycol groups high molecular material are 500~4000.
8. the preparation method of induced by magnetic field patterning assembling and erasable magnetic control phase-change material according to claim 4,
It is characterized in that, in step (1), the modified superparamagnetic nanomaterial of the surface nonpolarity the preparation method comprises the following steps: to super suitable
Magnetic Nano material surface is pre-processed, and introduces epoxy group on its surface；Then nonpolar long-chain Amino End Group modified
It is grafted to pretreatment gained particle surface, obtains the modified superparamagnetic nanomaterial of surface nonpolarity.
9. the preparation method of induced by magnetic field patterning assembling and erasable magnetic control phase-change material according to claim 8,
It is characterized in that, the preparation step for the superparamagnetic nanomaterial that the surface nonpolarity is modified includes:
It is to change with γ-glycidyl ether oxygen propyl trimethoxy silicane 1. superparamagnetic nanomaterial is added in ethanol solution
Property agent, reacted 2~3 hours at 65~80 DEG C, after reaction use ethanol washing, drying, obtain surface introduce epoxy group
Superparamagnetic nanomaterial；
2. by after drying product be added n,N-Dimethylformamide in, be added long chain alkane amine, at 60~80 DEG C react 3~
5 hours, Magneto separate, was washed with carbon tetrachloride solution after reaction, removed super-paramagnetism nano surface unmodified in product
Material to get.
10. the preparation method of induced by magnetic field patterning assembling and erasable magnetic control phase-change material according to claim 4,
It is characterized in that, polarity or nonpolar low temperature phase change macromolecule to be heated to 10 DEG C higher than its fusing point or more of temperature in step (2)
It spends, the superparamagnetic nanomaterial that surface polarity or nonpolarity are modified then is added, what the surface polarity or nonpolarity were modified
The additional amount of superparamagnetic nanomaterial is the 20~50% of polarity or nonpolar low temperature phase change high molecule mass.
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