CN109608912A - A method of improving dispersibility of the nanometer ferrite in magnetic ink - Google Patents
A method of improving dispersibility of the nanometer ferrite in magnetic ink Download PDFInfo
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- CN109608912A CN109608912A CN201910065387.1A CN201910065387A CN109608912A CN 109608912 A CN109608912 A CN 109608912A CN 201910065387 A CN201910065387 A CN 201910065387A CN 109608912 A CN109608912 A CN 109608912A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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Abstract
The present invention relates to the technical fields of magnetic ink, provide a kind of dispersed method for improving nanometer ferrite in magnetic ink.This method first passes through hydro-thermal reaction and carries out hydroxylating modification to nanometer ferrite, then fatty acid modifying is carried out to micron graphite piece, the reacting using hydroxyl and carboxyl under magnetic fields again, hydroxyl modified nanometer ferrite is carried on to the surface of fatty acid modifying micron graphite piece, graphite flake is made and loads Ferrite Material, it is added gained composite material as magnetic paint in ink, that is, can reach improves the purpose that compatibility, raising nanometer ferrite dispersibility and reduction between ferrite and organic linking material are reunited.
Description
Technical field
The invention belongs to the technical fields of magnetic ink, provide a kind of raising nanometer ferrite dividing in magnetic ink
Dissipate the method for property.
Background technique
Magnetic ink is selecting ink made of magnetizable material, mainly by pigment, binder, filler material and attached
Charging composition, wherein magnetizable material is primarily referred to as magnetic paint.Magnetic paint easily accomplishes that band magnetic arranges through magnetic field processing,
Higher residual magnetic is obtained, manufactured ink shows magnetism after being added in ink, becomes magnetic ink.Magnetic paint is in bank
The classification of ticket and postal service, retrieval, identification and field of anti-counterfeit technology have a wide range of applications.
In currently used magnetic paint, ferrite is a kind of metal oxide with ferrimagnetism, can according to magnetism
It is divided into soft magnetic materials and hard magnetic material, mainly there is spinel type ferrite, magneto-plumbite type ferrite, garnet according to lattice types
Type ferrite three classes.With resistivity, high, magnetic conductivity and magnetic susceptibility are big, high frequency magnetic conductivity is high, machining property is high for ferrite,
It is easy to the features such as pressing mold forms, chemical stability is good, at low cost, thus is concerned.
With the development of Nanometer scale science and technology, nano material has the quantum ruler that many traditional materials can not match in excellence or beauty because of it
The characteristics such as very little effect, small-size effect, skin effect and macro quanta tunnel effect and be concerned.Ferrite Material is in nanometer
There is excellent superparamagnetism, high-coercive force, lower Curie temperature on scale, therefore have a good application prospect.But
Due to nano material partial size is small and large specific surface area, there are nano effect, bad dispersibility, it is more easy to reunite to compare micro particles, system
The about application of nanometer ferrite.
In addition, when ferrite is used for magnetic ink as magnetic fillers, since ferrite is inorganic material, and in ink
Binder be organic synthetic resin, as alkyd resin, polyurethane resin, epoxy resin, polyvinyl acetate resins,
Polyvinyl butyral resin, polyvinyl ethyl ether resin, NC Nitroncellulose, polyurethane resin etc., because inorganic material with it is organic
Poor compatibility between material further promotes reunion of the ferrite in magnetic ink.
Therefore, when preparing magnetic ink using nanometer ferrite as magnetic paint, there are ferrite and organic linking material it
Between poor compatibility, nanometer ferrite bad dispersibility, defect easy to reunite.It finds technological means and overcomes drawbacks described above, there is weight
The meaning wanted.
Summary of the invention
As it can be seen that when preparing magnetic ink using nanometer ferrite as magnetic paint, there are ferrite and organic linking material it
Between poor compatibility, nanometer ferrite bad dispersibility, defect easy to reunite.In response to this, the present invention proposes a kind of raising
The method of dispersibility of the nanometer ferrite in magnetic ink, can reach compatible between improvement ferrite and organic linking material
Property, improve nanometer ferrite dispersibility and prevent reunite purpose.
To achieve the above object, specific technical solution of the present invention is as follows:
A method of improving dispersibility of the nanometer ferrite in magnetic ink, the tool for improving nanometer ferrite dispersibility
Steps are as follows for body:
(1) sodium hydroxide, iron chloride, frerrous chloride are added to the in the mixed solvent of glycerine and water, Nanoscale Iron oxygen is then added
Body, dispersing agent, 20 ~ 30min of ultrasonic disperse, then move into hydrothermal reaction kettle and are reacted, and are filtered, wash after reaction
It washs, and is dried in vacuo 8 ~ 12h at 70 ~ 80 DEG C, hydroxyl modified nanometer ferrite is made；
(2) long chain fatty acids are dissolved in ethyl alcohol, simultaneously 10 ~ 20min of ultrasonic disperse is added in deionized water in micron graphite piece, with
The speed of 80 ~ 120r/min is stirred graphite flake suspension, and the ethanol solution of fatty acid is then slowly dropped into suspension
In, continue 2 ~ 3h of stirring, filter, 4 ~ 6h is dried in vacuo at 40 ~ 50 DEG C, fatty acid modifying micron graphite piece is made；
(3) by fatty acid modifying micron graphite piece made from hydroxyl modified nanometer ferrite made from step (1), step (2), right
Toluenesulfonic acid is added in hexamethylene, and 20 ~ 30min of ultrasonic disperse forms suspension, is then heated to 78 ~ 82 DEG C and flow back instead
It answers, and magnetic field is applied to suspension, so that nanometer ferrite is carried on micron graphite piece surface with reacting for carboxyl by hydroxyl, and
Uniform sequential arrangement is formed under magnetic fields, stops heating after 50 ~ 60min, cooled to room temperature, be then filtered,
Washing, and 12 ~ 18h is dried in vacuo at 40 ~ 50 DEG C, graphite flake is made and loads Ferrite Material；
(4) it loads ferrite as magnetic paint using graphite flake made from step (3) to be added in ink, that is, can reach improves iron oxygen
Compatibility, raising nanometer ferrite dispersibility between body and organic linking material and the purpose for preventing reunion.
Preferably, the parts by weight of step (1) each raw material are, 3 ~ 5 parts by weight of sodium hydroxide, 2 ~ 4 parts by weight of iron chloride,
2 ~ 3 parts by weight of frerrous chloride, 31 ~ 52 parts by weight of glycerine, 20 ~ 30 parts by weight of water, 20 ~ 25 parts by weight of nanometer ferrite, dispersion
1 ~ 2 parts by weight of agent.
Preferably, step (1) nanometer ferrite is cubic system spinel type ferrite or hexagonal magneto-plumbite type sections
Oxysome, including but not limited to CoFeO4、ZnFeO4、MnFeO4、Co0.5Zn0.5FeO4、Mn0.5Zn0.5FeO4、BaFe12O19、
SrFe12O19、BaZn2Fe16O27、SrZn2Fe16O27；The nanometer ferrite is spherical, sheet or needle-shaped.
Preferably, step (1) dispersing agent is calgon, sodium pyrophosphate, sodium methylene bis-naphthalene sulfonate, methylene
One of double methyl naphthalene sulfonic acid sodium.
Preferably, the temperature of step (1) described hydro-thermal reaction is 150 ~ 160 DEG C, and the time is 4 ~ 6h.
Preferably, the parts by weight of step (2) each raw material are 1 ~ 2 parts by weight of long chain fatty acids, 20 ~ 30 weight of ethyl alcohol
Part, 8 ~ 12 parts by weight of micron graphite piece, 56 ~ 71 parts by weight of deionized water.
Preferably, step (2) long chain fatty acids are palmitinic acid, stearic acid, oleic acid, linoleic acid, alpha-linolenic acid, peanut
One of tetraenoic acid.
Preferably, the rate of addition of the ethanol solution of step (2) described fatty acid is 60 ~ 90 drops/min.
Preferably, the parts by weight of step (3) each raw material are 15 ~ 20 parts by weight of hydroxyl modified nanometer ferrite, fat
Acid modification 15 ~ 20 parts by weight of micron graphite piece, 1 ~ 2 parts by weight of p-methyl benzenesulfonic acid, 58 ~ 69 parts by weight of hexamethylene.
Preferably, the intensity in step (3) described magnetic field is 5000 ~ 7000Oe.
The present invention provides a kind of method of dispersibility of raising nanometer ferrite in magnetic ink, the feature protruded
It is with excellent effect:
1. method of the invention loads nanoscale ferrite with micron-sized graphite flake, pass through hydroxyl and carboxyl
Reaction makes to form chemical bonding between nanometer ferrite and graphite flake, has not only remained the advantage of particle nano-scale structure, but also gram
The shortcomings that easily reuniting between nanoparticle due to nano effect is taken.Also, by applying externally-applied magnetic field in loading process,
Nanometer ferrite is set to carry out orientations, thus obtained graphite flake/ferrite compound particle can also save after magnetization
It is magnetic.
2. method of the invention modifies micron graphite piece with long chain fatty acids, obtained graphite flake load iron oxygen
The surface of body material has long chain organic radical, can improve the compatibility between inorganic magnetic pigment and organic linking material, into one
Step promotes the evenly dispersed of magnetic paint.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
(1) sodium hydroxide, iron chloride, frerrous chloride are added to the in the mixed solvent of glycerine and water, Nanoscale Iron oxygen is then added
Body, dispersing agent, ultrasonic disperse 26min, then move into hydrothermal reaction kettle and are reacted, and are filtered, wash after reaction,
And it is dried in vacuo 11h at 74 DEG C, hydroxyl modified nanometer ferrite is made；The parts by weight of each raw material are 4 weight of sodium hydroxide
Part, 3 parts by weight of iron chloride, 2 parts by weight of frerrous chloride, 45 parts by weight of glycerine, 24 parts by weight of water, 23 weight of nanometer ferrite
Part, 1 parts by weight of dispersing agent；Nanometer ferrite is spherical CoFeO4；Dispersing agent is calgon；The temperature of hydro-thermal reaction is
156 DEG C, time 5h；
(2) long chain fatty acids are dissolved in ethyl alcohol, simultaneously ultrasonic disperse 14min is added in deionized water in micron graphite piece, with
The speed of 110r/min is stirred graphite flake suspension, and then the ethanol solution of fatty acid is slowly dropped into suspension,
Continue to stir 2.5h, filter, be dried in vacuo 5h at 46 DEG C, fatty acid modifying micron graphite piece is made；The parts by weight of each raw material are,
1 parts by weight of long chain fatty acids, 24 parts by weight of ethyl alcohol, 10 parts by weight of micron graphite piece, 65 parts by weight of deionized water；Long chain fatty acids
For palmitinic acid；The rate of addition of the ethanol solution of fatty acid is 70 drops/min；
(3) by fatty acid modifying micron graphite piece made from hydroxyl modified nanometer ferrite made from step (1), step (2), right
Toluenesulfonic acid is added in hexamethylene, and ultrasonic disperse 24min forms suspension, is then heated to 80 DEG C of progress back flow reactions, and right
Suspension applies magnetic field, so that nanometer ferrite is carried on micron graphite piece surface with reacting for carboxyl by hydroxyl, and in magnetic field
Uniform sequential arrangement is formed under effect, stops heating after 54min, then cooled to room temperature is filtered, washs, and
It is dried in vacuo 14h at 44 DEG C, graphite flake is made and loads Ferrite Material；The parts by weight of each raw material are hydroxyl modified Nanoscale Iron oxygen
17 parts by weight of body, 17 parts by weight of fatty acid modifying micron graphite piece, 1 parts by weight of p-methyl benzenesulfonic acid, 65 parts by weight of hexamethylene；Magnetic field
Intensity be 5800Oe；
(4) it loads ferrite as magnetic paint using graphite flake made from step (3) to be added in ink, that is, can reach improves iron oxygen
Compatibility, raising nanometer ferrite dispersibility between body and organic linking material and the purpose for reducing reunion.
Ink made from embodiment 1 is spread evenly across in glass slide, observation sample is made, electricity is scanned using SEM
Sem observation, it is seen that nanometer ferrite is uniformly dispersed in ink, soilless sticking phenomenon.
Embodiment 2
(1) sodium hydroxide, iron chloride, frerrous chloride are added to the in the mixed solvent of glycerine and water, Nanoscale Iron oxygen is then added
Body, dispersing agent, 20 ~ 30min of ultrasonic disperse, then move into hydrothermal reaction kettle and are reacted, and are filtered, wash after reaction
It washs, and is dried in vacuo 11h at 72 DEG C, hydroxyl modified nanometer ferrite is made；The parts by weight of each raw material are sodium hydroxide 3.5
Parts by weight, 2.5 parts by weight of iron chloride, 2 parts by weight of frerrous chloride, 47 parts by weight of glycerine, 23 parts by weight of water, nanometer ferrite 21
Parts by weight, 1 parts by weight of dispersing agent；Nanometer ferrite is sheet ZnFeO；Dispersing agent is sodium pyrophosphate；The temperature of hydro-thermal reaction is
153 DEG C, time 5.5h；
(2) long chain fatty acids are dissolved in ethyl alcohol, simultaneously ultrasonic disperse 12min is added in deionized water in micron graphite piece, with
The speed of 90r/min is stirred graphite flake suspension, and then the ethanol solution of fatty acid is slowly dropped into suspension, after
Continuous stirring 2h, filters, is dried in vacuo 5.5h at 42 DEG C, fatty acid modifying micron graphite piece is made；The parts by weight of each raw material are, long
1 parts by weight of chain fatty acid, 23 parts by weight of ethyl alcohol, 9 parts by weight of micron graphite piece, 68 parts by weight of deionized water；Long chain fatty acids are
Stearic acid；The rate of addition of the ethanol solution of fatty acid is 70 drops/min；
(3) by fatty acid modifying micron graphite piece made from hydroxyl modified nanometer ferrite made from step (1), step (2), right
Toluenesulfonic acid is added in hexamethylene, and ultrasonic disperse 22min forms suspension, is then heated to 79 DEG C of progress back flow reactions, and right
Suspension applies magnetic field, so that nanometer ferrite is carried on micron graphite piece surface with reacting for carboxyl by hydroxyl, and in magnetic field
Uniform sequential arrangement is formed under effect, stops heating after 53min, then cooled to room temperature is filtered, washs, and
It is dried in vacuo 16h at 42 DEG C, graphite flake is made and loads Ferrite Material；The parts by weight of each raw material are hydroxyl modified Nanoscale Iron oxygen
16 parts by weight of body, 16 parts by weight of fatty acid modifying micron graphite piece, 1 parts by weight of p-methyl benzenesulfonic acid, 67 parts by weight of hexamethylene；Magnetic field
Intensity be 5500Oe；
(4) it loads ferrite as magnetic paint using graphite flake made from step (3) to be added in ink, that is, can reach improves iron oxygen
Compatibility, raising nanometer ferrite dispersibility between body and organic linking material and the purpose for reducing reunion.
Ink made from embodiment 1 is spread evenly across in glass slide, observation sample is made, electricity is scanned using SEM
Sem observation, it is seen that nanometer ferrite is uniformly dispersed in ink, soilless sticking phenomenon.
Embodiment 3
(1) sodium hydroxide, iron chloride, frerrous chloride are added to the in the mixed solvent of glycerine and water, Nanoscale Iron oxygen is then added
Body, dispersing agent, ultrasonic disperse 28min, then move into hydrothermal reaction kettle and are reacted, and are filtered, wash after reaction,
And it is dried in vacuo 9h at 78 DEG C, hydroxyl modified nanometer ferrite is made；The parts by weight of each raw material are 4.5 weight of sodium hydroxide
Part, 3.5 parts by weight of iron chloride, 3 parts by weight of frerrous chloride, 35 parts by weight of glycerine, 28 parts by weight of water, 24 weight of nanometer ferrite
Part, 1 ~ 2 parts by weight of dispersing agent；Nanometer ferrite is needle-shaped MnFeO4；Dispersing agent is sodium methylene bis-naphthalene sulfonate；Hydro-thermal reaction
Temperature is 158 DEG C, time 4.5h；
(2) long chain fatty acids are dissolved in ethyl alcohol, simultaneously ultrasonic disperse 18min is added in deionized water in micron graphite piece, with
The speed of 110r/min is stirred graphite flake suspension, and then the ethanol solution of fatty acid is slowly dropped into suspension,
Continue to stir 2h, filter, be dried in vacuo 4.5h at 48 DEG C, fatty acid modifying micron graphite piece is made；The parts by weight of each raw material are,
2 parts by weight of long chain fatty acids, 27 parts by weight of ethyl alcohol, 11 parts by weight of micron graphite piece, 60 parts by weight of deionized water；Long chain fatty acids
For oleic acid；The rate of addition of the ethanol solution of fatty acid is 80 drops/min；
(3) by fatty acid modifying micron graphite piece made from hydroxyl modified nanometer ferrite made from step (1), step (2), right
Toluenesulfonic acid is added in hexamethylene, and ultrasonic disperse 28min forms suspension, is then heated to 81 DEG C of progress back flow reactions, and right
Suspension applies magnetic field, so that nanometer ferrite is carried on micron graphite piece surface with reacting for carboxyl by hydroxyl, and in magnetic field
Uniform sequential arrangement is formed under effect, stops heating after 58min, then cooled to room temperature is filtered, washs, and
It is dried in vacuo 14h at 48 DEG C, graphite flake is made and loads Ferrite Material；The parts by weight of each raw material are hydroxyl modified Nanoscale Iron oxygen
18 parts by weight of body, 19 parts by weight of fatty acid modifying micron graphite piece, 2 parts by weight of p-methyl benzenesulfonic acid, 61 parts by weight of hexamethylene；Magnetic field
Intensity be 6500Oe；
(4) it loads ferrite as magnetic paint using graphite flake made from step (3) to be added in ink, that is, can reach improves iron oxygen
Compatibility, raising nanometer ferrite dispersibility between body and organic linking material and the purpose for reducing reunion.
Ink made from embodiment 1 is spread evenly across in glass slide, observation sample is made, electricity is scanned using SEM
Sem observation, it is seen that nanometer ferrite is uniformly dispersed in ink, soilless sticking phenomenon.
Embodiment 4
(1) sodium hydroxide, iron chloride, frerrous chloride are added to the in the mixed solvent of glycerine and water, Nanoscale Iron oxygen is then added
Body, dispersing agent, ultrasonic disperse 20min, then move into hydrothermal reaction kettle and are reacted, and are filtered, wash after reaction,
And it is dried in vacuo 12h at 70 DEG C, hydroxyl modified nanometer ferrite is made；The parts by weight of each raw material are 3 weight of sodium hydroxide
Part, 2 parts by weight of iron chloride, 2 parts by weight of frerrous chloride, 52 parts by weight of glycerine, 20 parts by weight of water, 20 weight of nanometer ferrite
Part, 1 parts by weight of dispersing agent；Nanometer ferrite is spherical Co0.5Zn0.5FeO4；Dispersing agent is dispersing agent MF；
The temperature of hydro-thermal reaction is 150 DEG C, time 6h；
(2) long chain fatty acids are dissolved in ethyl alcohol, simultaneously ultrasonic disperse 10min is added in deionized water in micron graphite piece, with
The speed of 80r/min is stirred graphite flake suspension, and then the ethanol solution of fatty acid is slowly dropped into suspension, after
Continuous stirring 3h, filters, is dried in vacuo 6h at 40 DEG C, fatty acid modifying micron graphite piece is made；The parts by weight of each raw material are long-chain
1 parts by weight of fatty acid, 20 parts by weight of ethyl alcohol, 8 parts by weight of micron graphite piece, 71 parts by weight of deionized water；Long chain fatty acids are Asia
Oleic acid；The rate of addition of the ethanol solution of fatty acid is 60 drops/min；
(3) by fatty acid modifying micron graphite piece made from hydroxyl modified nanometer ferrite made from step (1), step (2), right
Toluenesulfonic acid is added in hexamethylene, and ultrasonic disperse 20min forms suspension, is then heated to 78 DEG C of progress back flow reactions, and right
Suspension applies magnetic field, so that nanometer ferrite is carried on micron graphite piece surface with reacting for carboxyl by hydroxyl, and in magnetic field
Uniform sequential arrangement is formed under effect, stops heating after 50min, then cooled to room temperature is filtered, washs, and
It is dried in vacuo 18h at 40 DEG C, graphite flake is made and loads Ferrite Material；The parts by weight of each raw material are hydroxyl modified Nanoscale Iron oxygen
15 parts by weight of body, 15 parts by weight of fatty acid modifying micron graphite piece, 1 parts by weight of p-methyl benzenesulfonic acid, 69 parts by weight of hexamethylene；Magnetic field
Intensity be 5000Oe；
(4) it loads ferrite as magnetic paint using graphite flake made from step (3) to be added in ink, that is, can reach improves iron oxygen
Compatibility, raising nanometer ferrite dispersibility between body and organic linking material and the purpose for reducing reunion.
Ink made from embodiment 1 is spread evenly across in glass slide, observation sample is made, electricity is scanned using SEM
Sem observation, it is seen that nanometer ferrite is uniformly dispersed in ink, soilless sticking phenomenon.
Embodiment 5
(1) sodium hydroxide, iron chloride, frerrous chloride are added to the in the mixed solvent of glycerine and water, Nanoscale Iron oxygen is then added
Body, dispersing agent, ultrasonic disperse 30min, then move into hydrothermal reaction kettle and are reacted, and are filtered, wash after reaction,
And it is dried in vacuo 8h at 80 DEG C, hydroxyl modified nanometer ferrite is made；The parts by weight of each raw material are, 5 parts by weight of sodium hydroxide,
4 parts by weight of iron chloride, 31 parts by weight of glycerine, 30 parts by weight of water, 25 parts by weight of nanometer ferrite, are divided at 3 parts by weight of frerrous chloride
2 parts by weight of powder；Nanometer ferrite is sheet Mn0.5Zn0.5FeO4；Dispersing agent is calgon；The temperature of hydro-thermal reaction is
160 DEG C, time 4h；
(2) long chain fatty acids are dissolved in ethyl alcohol, simultaneously ultrasonic disperse 20min is added in deionized water in micron graphite piece, with
The speed of 120r/min is stirred graphite flake suspension, and then the ethanol solution of fatty acid is slowly dropped into suspension,
Continue to stir 2h, filter, be dried in vacuo 4h at 50 DEG C, fatty acid modifying micron graphite piece is made；The parts by weight of each raw material are, long
2 parts by weight of chain fatty acid, 30 parts by weight of ethyl alcohol, 12 parts by weight of micron graphite piece, 56 parts by weight of deionized water；Long chain fatty acids are
Alpha-linolenic acid；The rate of addition of the ethanol solution of fatty acid is 90 drops/min；
(3) by fatty acid modifying micron graphite piece made from hydroxyl modified nanometer ferrite made from step (1), step (2), right
Toluenesulfonic acid is added in hexamethylene, and ultrasonic disperse 30min forms suspension, is then heated to 82 DEG C of progress back flow reactions, and right
Suspension applies magnetic field, so that nanometer ferrite is carried on micron graphite piece surface with reacting for carboxyl by hydroxyl, and in magnetic field
Uniform sequential arrangement is formed under effect, stops heating after 60min, then cooled to room temperature is filtered, washs, and
It is dried in vacuo 12h at 50 DEG C, graphite flake is made and loads Ferrite Material；The parts by weight of each raw material are hydroxyl modified Nanoscale Iron oxygen
20 parts by weight of body, 20 parts by weight of fatty acid modifying micron graphite piece, 2 parts by weight of p-methyl benzenesulfonic acid, 58 parts by weight of hexamethylene；Magnetic field
Intensity be 7000Oe；
(4) it loads ferrite as magnetic paint using graphite flake made from step (3) to be added in ink, that is, can reach improves iron oxygen
Compatibility, raising nanometer ferrite dispersibility between body and organic linking material and the purpose for reducing reunion.
Ink made from embodiment 1 is spread evenly across in glass slide, observation sample is made, electricity is scanned using SEM
Sem observation, it is seen that nanometer ferrite is uniformly dispersed in ink, soilless sticking phenomenon.
Embodiment 6
(1) sodium hydroxide, iron chloride, frerrous chloride are added to the in the mixed solvent of glycerine and water, Nanoscale Iron oxygen is then added
Body, dispersing agent, ultrasonic disperse 25min, then move into hydrothermal reaction kettle and are reacted, and are filtered, wash after reaction,
And it is dried in vacuo 10h at 75 DEG C, hydroxyl modified nanometer ferrite is made；The parts by weight of each raw material are 4 weight of sodium hydroxide
Part, 3 parts by weight of iron chloride, 3 parts by weight of frerrous chloride, 42 parts by weight of glycerine, 25 parts by weight of water, 22 weight of nanometer ferrite
Part, 1 parts by weight of dispersing agent；Nanometer ferrite is needle-shaped SrFe12O19；Dispersing agent is sodium pyrophosphate；The temperature of hydro-thermal reaction is
155 DEG C, time 5h；
(2) long chain fatty acids are dissolved in ethyl alcohol, simultaneously ultrasonic disperse 15min is added in deionized water in micron graphite piece, with
The speed of 100r/min is stirred graphite flake suspension, and then the ethanol solution of fatty acid is slowly dropped into suspension,
Continue to stir 2.5h, filter, be dried in vacuo 5h at 45 DEG C, fatty acid modifying micron graphite piece is made；The parts by weight of each raw material are,
2 parts by weight of long chain fatty acids, 25 parts by weight of ethyl alcohol, 10 parts by weight of micron graphite piece, 63 parts by weight of deionized water；Long chain fatty acids
For arachidonic acid；The rate of addition of the ethanol solution of fatty acid is 80 drops/min；
(3) by fatty acid modifying micron graphite piece made from hydroxyl modified nanometer ferrite made from step (1), step (2), right
Toluenesulfonic acid is added in hexamethylene, and ultrasonic disperse 25min forms suspension, is then heated to 80 DEG C of progress back flow reactions, and right
Suspension applies magnetic field, so that nanometer ferrite is carried on micron graphite piece surface with reacting for carboxyl by hydroxyl, and in magnetic field
Uniform sequential arrangement is formed under effect, stops heating after 55min, then cooled to room temperature is filtered, washs, and
It is dried in vacuo 15h at 45 DEG C, graphite flake is made and loads Ferrite Material；The parts by weight of each raw material are hydroxyl modified Nanoscale Iron oxygen
18 parts by weight of body, 18 parts by weight of fatty acid modifying micron graphite piece, 1 parts by weight of p-methyl benzenesulfonic acid, 63 parts by weight of hexamethylene；Magnetic field
Intensity be 6000Oe；
(4) it loads ferrite as magnetic paint using graphite flake made from step (3) to be added in ink, that is, can reach improves iron oxygen
Compatibility, raising nanometer ferrite dispersibility between body and organic linking material and the purpose for reducing reunion.
Ink made from embodiment 1 is spread evenly across in glass slide, observation sample is made, electricity is scanned using SEM
Sem observation, it is seen that nanometer ferrite is uniformly dispersed in ink, soilless sticking phenomenon.
Comparative example 1
Directly it is added nanometer ferrite as magnetic paint in ink.
Ink made from comparative example 1 is spread evenly across in glass slide, observation sample is made, electricity is scanned using SEM
Sem observation, it is seen that nanometer ferrite disperses unevenly in ink, and there are obvious agglomerations.
Claims (10)
1. a kind of dispersed method for improving nanometer ferrite in magnetic ink, which is characterized in that the raising Nanoscale Iron
Specific step is as follows for oxysome dispersibility:
(1) sodium hydroxide, iron chloride, frerrous chloride are added to the in the mixed solvent of glycerine and water, Nanoscale Iron oxygen is then added
Body, dispersing agent, 20 ~ 30min of ultrasonic disperse, then move into hydrothermal reaction kettle and are reacted, and are filtered, wash after reaction
It washs, and is dried in vacuo 8 ~ 12h at 70 ~ 80 DEG C, hydroxyl modified nanometer ferrite is made；
(2) long chain fatty acids are dissolved in ethyl alcohol, simultaneously 10 ~ 20min of ultrasonic disperse is added in deionized water in micron graphite piece, with
The speed of 80 ~ 120r/min is stirred graphite flake suspension, and the ethanol solution of fatty acid is then slowly dropped into suspension
In, continue 2 ~ 3h of stirring, filter, 4 ~ 6h is dried in vacuo at 40 ~ 50 DEG C, fatty acid modifying micron graphite piece is made；
(3) by fatty acid modifying micron graphite piece made from hydroxyl modified nanometer ferrite made from step (1), step (2), right
Toluenesulfonic acid is added in hexamethylene, and 20 ~ 30min of ultrasonic disperse forms suspension, is then heated to 78 ~ 82 DEG C and flow back instead
It answers, and magnetic field is applied to suspension, so that nanometer ferrite is carried on micron graphite piece surface with reacting for carboxyl by hydroxyl, and
Uniform sequential arrangement is formed under magnetic fields, stops heating after 50 ~ 60min, cooled to room temperature, be then filtered,
Washing, and 12 ~ 18h is dried in vacuo at 40 ~ 50 DEG C, graphite flake is made and loads Ferrite Material；
(4) it loads ferrite as magnetic paint using graphite flake made from step (3) to be added in ink, that is, can reach improves iron oxygen
Compatibility, raising nanometer ferrite dispersibility between body and organic linking material and the purpose for reducing reunion.
2. a kind of dispersed method for improving nanometer ferrite in magnetic ink, feature exist according to claim 1
In: the parts by weight of step (1) each raw material are 3 ~ 5 parts by weight of sodium hydroxide, 2 ~ 4 parts by weight of iron chloride, frerrous chloride 2 ~ 3
Parts by weight, 31 ~ 52 parts by weight of glycerine, 20 ~ 30 parts by weight of water, 20 ~ 25 parts by weight of nanometer ferrite, 1 ~ 2 parts by weight of dispersing agent.
3. a kind of dispersed method for improving nanometer ferrite in magnetic ink, feature exist according to claim 1
In: step (1) nanometer ferrite be cubic system spinel type ferrite or hexagonal magneto-plumbite type ferrite, including but not
It is limited to CoFeO4、ZnFeO4、MnFeO4、Co0.5Zn0.5FeO4、Mn0.5Zn0.5FeO4、BaFe12O19、SrFe12O19、
BaZn2Fe16O27、SrZn2Fe16O27；The nanometer ferrite is spherical, sheet or needle-shaped.
4. a kind of dispersed method for improving nanometer ferrite in magnetic ink, feature exist according to claim 1
In: step (1) dispersing agent is calgon, sodium pyrophosphate, sodium methylene bis-naphthalene sulfonate, di-2-ethylhexylphosphine oxide methyl naphthalene sulfonic acid
One of sodium.
5. a kind of dispersed method for improving nanometer ferrite in magnetic ink, feature exist according to claim 1
In: the temperature of step (1) described hydro-thermal reaction is 150 ~ 160 DEG C, and the time is 4 ~ 6h.
6. a kind of dispersed method for improving nanometer ferrite in magnetic ink, feature exist according to claim 1
In: the parts by weight of step (2) each raw material are 1 ~ 2 parts by weight of long chain fatty acids, 20 ~ 30 parts by weight of ethyl alcohol, micron graphite piece
8 ~ 12 parts by weight, 56 ~ 71 parts by weight of deionized water.
7. a kind of dispersed method for improving nanometer ferrite in magnetic ink, feature exist according to claim 1
In: step (2) long chain fatty acids be palmitinic acid, stearic acid, oleic acid, linoleic acid, alpha-linolenic acid, one in arachidonic acid
Kind.
8. a kind of dispersed method for improving nanometer ferrite in magnetic ink, feature exist according to claim 1
In: the rate of addition of the ethanol solution of step (2) described fatty acid is 60 ~ 90 drops/min.
9. a kind of dispersed method for improving nanometer ferrite in magnetic ink, feature exist according to claim 1
In: the parts by weight of step (3) each raw material are 15 ~ 20 parts by weight of hydroxyl modified nanometer ferrite, fatty acid modifying micron stone
15 ~ 20 parts by weight of ink sheet, 1 ~ 2 parts by weight of p-methyl benzenesulfonic acid, 58 ~ 69 parts by weight of hexamethylene.
10. a kind of dispersed method for improving nanometer ferrite in magnetic ink, feature exist according to claim 1
In: the intensity in step (3) described magnetic field is 5000 ~ 7000Oe.
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