CN109206557A - A kind of preparation method of black high molecule magnetic microsphere - Google Patents
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- C—CHEMISTRY; METALLURGY
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F257/00—Macromolecular compounds obtained by polymerising monomers on to polymers of aromatic monomers as defined in group C08F12/00
- C08F257/02—Macromolecular compounds obtained by polymerising monomers on to polymers of aromatic monomers as defined in group C08F12/00 on to polymers of styrene or alkyl-substituted styrenes
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/22—Oxides; Hydroxides of metals
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- 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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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Abstract
The invention discloses a kind of preparation methods of black high molecule magnetic microsphere.By adding the uniform black high molecule magnetic microsphere of magnetisable material preparation property in black polymer microsphere, induction well can be generated in the electric field, so that blur-free imaging, solves the problem of power consumption is big, and the imaging is not clear in Electronic Paper imaging.
Description
Technical field
The present invention relates to a kind of preparation method of black high molecule magnetic microsphere, belong to micro- containing the high molecular magnetism of black
The technical field of ball preparation method.
Background technique
With the development of electronic paper display technology, based on the display device of electronic paper technology towards in bright gay colorization, ultra-thin
Change, energy-saving development.
Electronics stationery display device generally comprises: upper substrate (silica gel piece or glass substrate) and lower substrate (silica gel piece or glass
Glass substrate), and liquid crystal layer or microballoon layer between upper substrate and lower substrate；Wherein, the upper substrate includes common electrical
Pole, the lower substrate include: thin film transistor (TFT) TFT, pixel electrode and reflecting layer；Pixel electrode receives data line according to TFT
Signal forms the electric field of variation between the upper substrate and lower substrate, makes liquid crystal layer or microballoon layer by the variation of electric field
Liquid crystal or microballoon change, and then display device is made to show image.
Based on electronic paper technology in the prior art mostly uses greatly black and white ink microballoon, this display device of electronic paper is adopted
With the transparent film similar with plain paper, it distributed quantity inside film and be up to the diameter of million meters in 100 microns
The electric globule of size, electric globule of the bubble internal in this way in lubricating oil will be rotated under the action of electric field, be selected
Property by black, perhaps white portion flips out and needs text to be shown or pattern macroscopically being formed.But this imaging
It tends not to clearly show, and more power consumption.
Liquid crystal display in order to obtain clearer display effect, needs evenly dispersed in liquid crystal material in process of production
Size is suitable, uniform particle diameter, the black polymer microsphere with high compression-strength and elasticity.
And the display device based on liquid crystal needs that light loss can be generated using color film, reduces light transmittance, it is therefore desirable to additional
Light source provide brightness, this will consume additional electricity.
If the black polymer microsphere for increasing clarity in liquid crystal display is prepared as magnetic microsphere, in the electric field
Induction well can be generated, thus blur-free imaging, solving the problem of power consumption, big the imaging is not clear.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of preparation methods of black high molecule magnetic microsphere.
Black high molecule magnetic microsphere, which is prepared, to achieve the effect that blur-free imaging under electric field induction.
In order to achieve the above objectives, the invention adopts the following technical scheme:
The embodiment of the invention provides a kind of preparation methods of black high molecule magnetic microsphere, including,
(1) synthesis of magnetic particle: at 70-90 DEG C, by soluble trivalent iron salt and enuatrol in n-hexane and ethyl alcohol
It reacts, is dried in vacuo in system, obtain dry iron oleate；
(2) synthesis of black monomer suspension: stabilizer/solvent is added in double bond containing black monomer and vinyl monomer and is mixed
It in solution, stirs evenly, forms black matrix monomer suspension;
(3) synthesis of initiator suspension:
Initiator is added in the aqueous solution containing stabilizer, emulsification forms initiator suspension；
(4) magnetic black monomer synthesis:
Iron oleate and black monomer suspension are added in stabilizer/solvent mixed solution, stirred evenly, iron oleate black is formed
Monomer suspension；
(5) polymer seeds synthesize:
Polymer is added in the aqueous solution containing dispersing agent, is sufficiently stirred, forms evenly dispersed seed suspension liquid, polymer
Seed accounts for 60% or less seed suspension liquid weight；
(6) cause polymerization:
At the polymerization temperature, iron oleate black monomer suspension and initiator are added in seed suspension liquid makes seed growth, reaches
Stop that iron oleate black monomer suspension and initiator is added after to preset microspherulite diameter, heat up polymerization reaction for the first time, i.e.,
Black iron oleate polymer composite microsphere can be obtained；Second of heating, makes iron oleate pyrolysis synthesizing magnetic nano particle,
Black high molecule magnetic microsphere can be obtained.
In above scheme, the initiator is persulfide.
In above scheme, the black monomer is that organic black dyes is included that step acylation reaction is obtained containing non-
The black monomer of phenyl ring carbon-carbon double bond.
In above scheme, the polymer seeds are polystyrene seed or styrene-divinylbenzene seed, the list
Body is selected from styrene, divinylbenzene, 2,4 dichloro benzene ethylene, acrylic acid, methyl methacrylate, methyl acrylate, acrylic acid
One of ethyl ester, vinylacetate, glycidyl methacrylate or derivatives thereof are a variety of.
In above scheme, solvent is the lower alcohol of C1-C3.
In above scheme, the temperature of heating is 95-110 DEG C for the first time, and the temperature of second of heating is 300-350 DEG C.
In above scheme, the particle size of black high molecule magnetic microsphere is 0.1-5000 μm.
In above scheme, the molar ratio of the solubility trivalent iron salt and enuatrol is 1:2-1:7.
In above scheme, organic black dyes is nigrosine.
In above scheme, the vinyl monomer is selected from divinylbenzene, methyl methacrylate, methyl acrylate, acrylic acid
One of ethyl ester, vinylacetate, ethylene glycol dimethacrylate, dimethacrylate.
In above scheme, the stabilizer is hydroxymethyl cellulose, hydroxypropyl cellulose or dextrin.
Advantageous effects of the invention:
Black high molecule magnetic microsphere uniform particle diameter that the present invention synthesizes, surface smooth, spherical degree are good, and grain diameter is easy to control,
And microballoon property is stablized, and has and stablizes magnetism, can achieve the effect that blur-free imaging under electric field induction, solve Electronic Paper imaging
The problem of middle power consumption is big, and the imaging is not clear.
Specific embodiment
The invention will be further described combined with specific embodiments below.Following embodiment is only used for clearly illustrating
Technical solution of the present invention, and not intended to limit the protection scope of the present invention.
Embodiment 1
A kind of black high molecule magnetic microsphere preparation method takes FeCl comprising steps of preparing dry iron oleate3With enuatrol plus
Enter in flask, and the mixed solution of dehydrated alcohol and n-hexane is added into flask, after dissolution, 80 DEG C of heating stirring 4h, filtering
Wet iron oleate is obtained, then wet iron oleate is placed in 80 DEG C, is dried for 24 hours in vacuum oven under conditions of vacuum degree is 100Pa,
Obtain dry iron oleate；Hydroxymethyl cellulose stabilizer and solvent is added in double bond containing black monomer and divinylbenzene monomers
It in mixed solution, stirs evenly, forms black matrix monomer suspension；In the stabilizer/solvent, solvent refers to that 60% ethyl alcohol is water-soluble
Liquid；Initiator potassium persulfate is added in the aqueous solution containing stabilizer, emulsification forms initiator suspension；By iron oleate and
Black monomer suspension is added in stabilizer/solvent mixed solution, stirs evenly, and forms iron oleate black monomer suspension；It will
It in (152 μm of granularity, CV=3%) aqueous solutions of the addition containing polyethylene glycol of styrene homopolymers seed, is sufficiently stirred, is formed equal
The seed suspension liquid of even dispersion, styrene homopolymers seed account for the 50% of seed suspension liquid weight；Dispersing agent polyethylene glycol weight
It is the 10% of styrene homopolymers seed weight；At 70 DEG C, by iron oleate black monomer suspension and initiation in 360 minutes
Agent suspension, which is added in seed suspension liquid, makes seed growth, wherein it is 6.8g/ that speed, which is added, in iron oleate black monomer suspension
Min, it is 1.01g/min that speed, which is added, in initiator suspension, after reaching preset microspherulite diameter stops that iron oleate black list is added
Liquid suspension and initiator suspension, are warming up to 110 DEG C, and the reaction was continued, and 30min is compound micro- to get black iron oleate polymer is arrived
Ball；It is warming up to 350 DEG C for the second time, and keeps 2-3h in the case where being kept for 350 DEG C, makes iron oleate pyrolysis synthesizing black macromolecule
Black magnetic polymer microballoon can be obtained in magnetic nanoparticle.Magnetic nanoparticle is ferroso-ferric oxide herein.Using
BeckmanCounter measures its partial size and particle diameter distribution obtains: partial size is 200 μm, and CV 2%, magnetic ferroferric oxide accounts for entirely
The 56% of microspheres weight.
Embodiment 2
A kind of black high molecule magnetic microsphere preparation method takes FeCl comprising steps of preparing dry iron oleate3With enuatrol plus
Enter in flask, and the mixed solution of dehydrated alcohol and n-hexane is added into flask, after dissolution, 80 DEG C of heating stirring 4h, filtering
Wet iron oleate is obtained, then wet iron oleate is placed in 80 DEG C, is dried for 24 hours in vacuum oven under conditions of vacuum degree is 100Pa,
Obtain dry iron oleate；By double bond containing black monomer and methyl methacrylate be added hydroxypropyl cellulose mix with solvent it is molten
It in liquid, stirs evenly, forms black matrix monomer suspension；In the stabilizer/solvent, solvent refers to 60% ethanol water；It will draw
It sends out agent potassium peroxydisulfate to be added in the aqueous solution containing stabilizer, emulsification forms initiator suspension；By iron oleate and black monomer
Suspension is added in stabilizer/solvent mixed solution, stirs evenly, and forms iron oleate black monomer suspension；By styrene-two
It in (200 μm of granularity, CV=3%) aqueous solutions of the addition containing polyethylene glycol of vinyl benzene seed, is sufficiently stirred, is formed and uniformly divided
Scattered seed suspension liquid, styrene homopolymers seed account for the 50% of seed suspension liquid weight；Dispersing agent polyethylene glycol weight is benzene
The 10% of Alathon seed weight；At 70 DEG C, iron oleate black monomer suspension and initiator are hanged in 360 minutes
Supernatant liquid, which is added in seed suspension liquid, makes seed growth, wherein it is 6.8g/min that speed, which is added, in iron oleate black monomer suspension, is drawn
Sending out agent suspension and speed is added is 1.01g/min, and stopping addition iron oleate black monomer suspends after reaching preset microspherulite diameter
Liquid and initiator suspension, are warming up to 95 DEG C, and the reaction was continued 30min is to get arriving black iron oleate polymer composite microsphere；Second
It is secondary to be warming up to 300 DEG C, and 2-3h is kept in the case where being kept for 350 DEG C, so that iron oleate pyrolysis synthesizing black High Polymer Magnetic is received
Black magnetic polymer microballoon can be obtained in rice grain.Magnetic nanoparticle is ferroso-ferric oxide herein.Using
BeckmanCounter measures its partial size and particle diameter distribution obtains: partial size is 1000 μm, and CV 5%, magnetic ferroferric oxide accounts for whole
The 60% of a microspheres weight.
Embodiment 3
A kind of black high molecule magnetic microsphere preparation method takes FeCl comprising steps of preparing dry iron oleate3With enuatrol plus
Enter in flask, and the mixed solution of dehydrated alcohol and n-hexane is added into flask, after dissolution, 80 DEG C of heating stirring 4h, filtering
Wet iron oleate is obtained, then wet iron oleate is placed in 80 DEG C, is dried for 24 hours in vacuum oven under conditions of vacuum degree is 100Pa,
Obtain dry iron oleate；Double bond containing black monomer and methyl acrylate are added in dextrin and solvent mixed solution, stirring is equal
It is even, form black matrix monomer suspension；In the stabilizer/solvent, solvent refers to 60% ethanol water；By initiator potassium persulfate
It is added in the aqueous solution containing stabilizer, emulsification forms initiator suspension；Iron oleate and black monomer suspension are added steady
Determine to stir evenly in agent/solvent mixed solution, forms iron oleate black monomer suspension；By styrene homopolymers seed (granularity
152 μm, CV=3%) it is added in the aqueous solution containing polyethylene glycol, it is sufficiently stirred, forms evenly dispersed seed suspension liquid, benzene
Alathon seed accounts for the 50% of seed suspension liquid weight；Dispersing agent polyethylene glycol weight is styrene homopolymers seed weight
10%；At 70 DEG C, seed suspension liquid is added in iron oleate black monomer suspension and initiator suspension in 360 minutes
In make seed growth, wherein iron oleate black monomer suspension be added speed be 6.8g/min, initiator suspension be added speed
For 1.01g/min, after reaching preset microspherulite diameter stops that iron oleate black monomer suspension and initiator suspension is added, rise
Temperature is to 100 DEG C, and the reaction was continued 30min is to get arriving black iron oleate polymer composite microsphere；It is warming up to 330 DEG C for the second time, and
It keeps keeping 2-3h at 350 DEG C, makes iron oleate pyrolysis synthesizing black High Polymer Magnetic nano particle, black can be obtained
Magnetic polymer microsphere.Magnetic nanoparticle is ferroso-ferric oxide herein.Its partial size and grain are measured using BeckmanCounter
Diameter is distributed: partial size is 4500 μm, and CV 3%, magnetic ferroferric oxide accounts for the 54% of entire microspheres weight.
Embodiment 4
A kind of black high molecule magnetic microsphere preparation method takes FeCl comprising steps of preparing dry iron oleate3With enuatrol plus
Enter in flask, and the mixed solution of dehydrated alcohol and n-hexane is added into flask, after dissolution, 80 DEG C of heating stirring 4h, filtering
Wet iron oleate is obtained, then wet iron oleate is placed in 80 DEG C, is dried for 24 hours in vacuum oven under conditions of vacuum degree is 100Pa,
Obtain dry iron oleate；Hydroxymethyl cellulose and solvent mixed solution is added in double bond containing black monomer and ethyl acrylate
In, it stirs evenly, forms black matrix monomer suspension；In the stabilizer/solvent, solvent refers to 60% ethanol water；It will cause
Agent potassium peroxydisulfate is added in the aqueous solution containing stabilizer, and emulsification forms initiator suspension；Iron oleate and black monomer are hanged
Supernatant liquid is added in stabilizer/solvent mixed solution, stirs evenly, and forms iron oleate black monomer suspension；By styrene homopolymerization
In species (0.05 μm of granularity, CV=3%) aqueous solution of the addition containing polyethylene glycol of son, it is sufficiently stirred, is formed evenly dispersed
Seed suspension liquid, styrene homopolymers seed account for the 50% of seed suspension liquid weight；Dispersing agent polyethylene glycol weight is styrene
The 10% of homopolymer seed weight；At 70 DEG C, by iron oleate black monomer suspension and initiator suspension in 360 minutes
Being added in seed suspension liquid makes seed growth, wherein it is 6.8g/min, initiator that speed, which is added, in iron oleate black monomer suspension
It is 1.01g/min that speed, which is added, in suspension, reach stop after preset microspherulite diameter being added iron oleate black monomer suspension and
Initiator suspension is warming up to 110 DEG C, and the reaction was continued 30min is to get arriving black iron oleate polymer composite microsphere；Second
300 DEG C are warming up to, and keeps 2-3h in the case where being kept for 350 DEG C, makes iron oleate pyrolysis synthesizing black High Polymer Magnetic nanometer
Black magnetic polymer microballoon can be obtained in particle.Magnetic nanoparticle is ferroso-ferric oxide herein.Using
BeckmanCounter measures its partial size and particle diameter distribution obtains: partial size is 0.2 μm, and CV 3%, magnetic ferroferric oxide accounts for entirely
The 55% of microspheres weight.
Embodiment 5
A kind of black high molecule magnetic microsphere preparation method takes FeCl comprising steps of preparing dry iron oleate3With enuatrol plus
Enter in flask, and the mixed solution of dehydrated alcohol and n-hexane is added into flask, after dissolution, 80 DEG C of heating stirring 4h, filtering
Wet iron oleate is obtained, then wet iron oleate is placed in 80 DEG C, is dried for 24 hours in vacuum oven under conditions of vacuum degree is 100Pa,
Obtain dry iron oleate；By double bond containing black monomer and divinylbenzene monomers be added hydroxyethyl cellulose mix with solvent it is molten
It in liquid, stirs evenly, forms black matrix monomer suspension；In the stabilizer/solvent, solvent refers to 60% ethanol water；It will draw
It sends out agent potassium peroxydisulfate to be added in the aqueous solution containing stabilizer, emulsification forms initiator suspension；By iron oleate and black monomer
Suspension is added in stabilizer/solvent mixed solution, stirs evenly, and forms iron oleate black monomer suspension；Styrene is equal
In (152 μm of granularity, CV=3%) aqueous solutions of the addition containing polyethylene glycol of polymers seed, it is sufficiently stirred, is formed evenly dispersed
Seed suspension liquid, styrene homopolymers seed account for the 50% of seed suspension liquid weight；Dispersing agent polyethylene glycol weight is styrene
The 10% of homopolymer seed weight；At 70 DEG C, by iron oleate black monomer suspension and initiator suspension in 360 minutes
Being added in seed suspension liquid makes seed growth, wherein it is 6.8g/min, initiator that speed, which is added, in iron oleate black monomer suspension
It is 1.01g/min that speed, which is added, in suspension, reach stop after preset microspherulite diameter being added iron oleate black monomer suspension and
Initiator suspension is warming up to 110 DEG C, and the reaction was continued 30min is to get arriving black iron oleate polymer composite microsphere；Second
310 DEG C are warming up to, and keeps 2-3h in the case where being kept for 350 DEG C, makes iron oleate pyrolysis synthesizing black High Polymer Magnetic nanometer
Black magnetic polymer microballoon can be obtained in particle.Magnetic nanoparticle is ferroso-ferric oxide herein.Using
BeckmanCounter measures its partial size and particle diameter distribution obtains: partial size is 250 μm, and CV 4%, magnetic ferroferric oxide accounts for entirely
The 58% of microspheres weight.
The above is only a preferred embodiment of the present invention, it is noted that those skilled in the art are come
It says, without departing from the technical principles of the invention, several improvement and deformations can also be made, these improvement and deformations are also answered
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of preparation method of black high molecule magnetic microsphere, feature include,
(1) synthesis of magnetic particle:
At 70-90 DEG C, soluble trivalent iron salt and enuatrol are reacted in the system of n-hexane and ethyl alcohol, vacuum is dry
It is dry, obtain dry iron oleate；
(2) synthesis of black monomer suspension:
Double bond containing black monomer and vinyl monomer are added in stabilizer/solvent mixed solution, stirred evenly, black matrix list is formed
Liquid suspension;
(3) synthesis of initiator suspension:
Initiator is added in the aqueous solution containing stabilizer, emulsification forms initiator suspension；
(4) magnetic black monomer synthesis:
Iron oleate and black monomer suspension are added in stabilizer/solvent mixed solution, stirred evenly, iron oleate black is formed
Monomer suspension；
(5) polymer seeds synthesize:
Polymer is added in the aqueous solution containing dispersing agent, is sufficiently stirred, forms evenly dispersed seed suspension liquid, polymer
Seed accounts for 60% or less seed suspension liquid weight；
(6) cause polymerization:
At the polymerization temperature, iron oleate black monomer suspension and initiator are added in seed suspension liquid makes seed growth, reaches
Stop that iron oleate black monomer suspension and initiator is added after to preset microspherulite diameter, heat up polymerization reaction for the first time, i.e.,
Black iron oleate polymer composite microsphere can be obtained；Second of heating, makes iron oleate pyrolysis synthesizing magnetic nano particle,
Black high molecule magnetic microsphere can be obtained.
2. preparation method according to claim 1, which is characterized in that the initiator is persulfide.
3. preparation method according to claim 2, which is characterized in that the black monomer is organic black dyes through including
The step acylation reaction black monomer obtained for containing non-phenyl ring carbon-carbon double bond.
4. preparation method according to claim 1-3, which is characterized in that the polymer seeds are polystyrene
Seed or styrene-divinylbenzene seed, the monomer are selected from styrene, divinylbenzene, 2,4- dichlorostyrene, propylene
Acid, methyl methacrylate, methyl acrylate, ethyl acrylate, vinylacetate, glycidyl methacrylate or its spread out
One of biology is a variety of.
5. preparation method according to claim 1 to 3, which is characterized in that solvent is the lower alcohol of C1-C3.
6. preparation method according to claim 1 or 5, which is characterized in that the temperature of heating is 95-110 DEG C for the first time, the
The temperature of secondary temperature elevation is 300-350 DEG C.
7. preparation method according to claim 1, which is characterized in that the particle size of black high molecule magnetic microsphere is
0.1-5000μm。
8. preparation method according to claim 1, which is characterized in that mole of the solubility trivalent iron salt and enuatrol
Than for 1:2-1:7.
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| CN110498879A (en) * | 2019-09-06 | 2019-11-26 | 苏州知益微球科技有限公司 | A kind of preparation method of black polymer microballoon |
| CN110511309A (en) * | 2019-09-06 | 2019-11-29 | 无锡迈科为生物科技有限公司 | A kind of preparation method of magnetic macromolecular microsphere |
| CN111995713A (en) * | 2020-07-24 | 2020-11-27 | 无锡迈科为生物科技有限公司 | Red polymer microsphere and preparation method thereof |
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| CN105754021A (en) * | 2016-05-18 | 2016-07-13 | 苏州知益微球科技有限公司 | Method for preparing mean-particle magnetic polymer microsphere |
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| CN110498879A (en) * | 2019-09-06 | 2019-11-26 | 苏州知益微球科技有限公司 | A kind of preparation method of black polymer microballoon |
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