CN106433289A - Preparation method for magnetic water-based ink with nano-gold magnetic powder - Google Patents
Preparation method for magnetic water-based ink with nano-gold magnetic powder Download PDFInfo
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- CN106433289A CN106433289A CN201610927232.0A CN201610927232A CN106433289A CN 106433289 A CN106433289 A CN 106433289A CN 201610927232 A CN201610927232 A CN 201610927232A CN 106433289 A CN106433289 A CN 106433289A
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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
- 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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- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention relates to magnetic water-based ink with nano-gold magnetic powder. The magnetic water-based ink comprises the following components in percent by weight: 2-4% of nano-gold magnetic powder and 96-98% of water-based ink. A method for the magnetic water-based ink with the nano-gold magnetic powder comprises the following steps of (S1) preparing Fe3O4 nanoparticles; (S2) preparing Fe3O4/Au nanoparticles; (S3) continuously reacting for 5-6 hours at the temperature of 80 DEG C, and after separation, washing with water for spare use; (S4) adding water-based colour paste, a solvent, a surface active agent and a corresponding additive into Fe3O4/Au powder till generating corresponding water-based ink. The magnetic water-based ink and the preparation method have the advantages that (1) the magnetic saturation degree is large, the size is uniform, the dispersity is good, the stability is strong, the timeliness is long, the coloring power is high and the color saturation degree is high; (2) the obvious defects of nano-size Fe3O4 as a permanent magnetic material, such as easy aggregation and loss of magnetism due to certain complex samples, can be overcome; and (3) a layer of Au housing is wrapped outside Fe3O4, so that effective protection for Fe3O4 can be realized.
Description
Technical field
The present invention relates to a kind of preparation method of water-based inks, belongs to organic chemical industry field.
Background technology
Water-based inks are called water color ink or aqueous ink again. and it is usually used in silk screen printing than ink environmental protection, silk-screen base
The waterproof nylon fabric that material cannot be printed for common nylon rubber cement or PU rubber cement, leather, PET PVC film, coating oxford, rain
Fabric of the spill resistant coating such as clothing, umbrella etc..
Water-based inks are formed through Compound Machining grinding by water-soluble resin, senior pigment, solvent and auxiliary agent.Water solublity tree
Fat acts primarily as the effect of binder in ink, makes granules of pigments dispersed, makes ink have certain mobility, produce with
The adhesion of stock material, makes ink form uniform film layer after printing.Form and aspect in ink depend primarily on pigment, face
Material is evenly distributed in binder with graininess, and granules of pigments can produce to light and absorb, reflects, reflecting and transmission
Effect, therefore, it is possible to assume certain color.Typically require that pigment has bright-coloured color and luster, appropriate tinting strength, tinting power and covering power, with
And higher dispersion.
Magnetic water-based inks select magnetizable pigment, such as iron oxide black (Fe3O4), iron oxide brown (Fe2O3), these grains
Son is mostly the acicular crystal less than 1 μm.Process through magnetic field and easily accomplish magnetic arrangement is carried, higher residual magnetic is obtained, is added
The ink that makes after in ink manifests magnetic, becomes magnetic ink.It bank's ticket and postal service classification, retrieve, distinguish
The aspect application such as recognize quite wide.Can be made into the kinds such as magnetic letterpress printing ink, magnetic offset lithography printing ink.But existing magnetic water-based inks is scarce
Point is, stability is poor, skewness rotten so as to cause of easily reuniting, and aberration sometimes occurs, so as to affect book
Write, printing quality.
Content of the invention
It is an object of the invention to provide a kind of preparation method of water-based inks, particularly a kind of based on Fe3O4The magnetic of/Au
Property water-based inks preparation method.
A kind of nanometer gold Magnetic Characteristics of Magnetic Particles water-based inks, by percentage by weight for 2-4% nanometer gold magnetic powder and 96%-98%
Water-based inks composition.
The water-based inks include the aqueous color paste of 22.5-26.5%, the polyurethane of 55-60%, the ethanol of 15-20%,
The surfactant of 2-5%, described solvent is ethanol, and described surfactant is organic silicon defoamer, organosilicon moistening
Dispersant and DBSA.
A kind of preparation method of nanometer gold Magnetic Characteristics of Magnetic Particles water-based inks, it is characterised in that comprise the steps：
S1, preparation Fe3O4Nanoparticle：By FeCl3·6H2O and FeCl2·4H2O is dissolved in 0.01M HCl, in stirring condition
Under, it is added dropwise in NaOH, whole Deca building-up process keeping temperature is 60-80 DEG C, and leads to N2Except O2And keep 2-4 little
Shi Zhizhi generates the precipitation of black；
S2, take above-mentioned Fe3O4Nanoparticle dilutes 15-20 times, adds sodium citrate, stirs under the rotating speed of 1000-3000rpm
Mixing uniformly, solution is heated to 60-80 DEG C, then the gold chloride of 0.15-0.2M oxammonium hydrochloride. and 1-3% is added dropwise over to solution
Color becomes laking by black；
S3, at 60-80 DEG C continue reaction 5-6 hour, with Magnet will synthesize Fe3O4/ Au nanoparticle is separated, and uses distilled water
Standby after washing 2-3 time；
S4, in the Fe for preparing3O4In/Au powder body, addition aqueous color paste, solvent, surfactant and corresponding auxiliary agent are until raw
Become corresponding water-based inks.
Lead to N in step S12Except O2And 2-4 hour is kept until generating the precipitation of black.
Step S1 prepares Fe3O4The Fe that will be synthesized with Magnet after nanoparticle3O4Nanoparticle is separated, and washes 2-3 with water
Secondary, it is dispersed in standby in five water of Tetramethylammonium hydroxide.
The preparation method of nanometer gold Magnetic Characteristics of Magnetic Particles water-based inks of the present invention, contrast prior art has excellent as follows
Point：
(1) magnetic saturation is big, uniform in size, good dispersion, and stability is strong, ageing length, tinting strength, tinting power height, color saturation height,
Gorgeous water-fast, wearability is good, and penetration power is strong；
(2) overcome the Fe of nano-scale3O4As some obvious shortcomings that a kind of permanent magnet material has, such as easily aggregation, certain
A little complex samples can cause which to lose magnetism；
(3) in Fe3O4Outer bread enclose layer of Au shell, can be achieved with to Fe3O4It is effectively protected.
Description of the drawings
Fig. 1 is schemed for the TEM of nanometer gold magnetic powder.
Specific embodiment
With reference to embodiment, nanometer gold Magnetic Characteristics of Magnetic Particles water-based inks of the present invention are described further, but this
The claimed scope of invention is not limited to the scope described in embodiment.
Embodiment 1：
(1)Fe3O4The preparation of nanoparticle, by 10.8g FeCl3·6H2O and 4.0g FeCl2·4H2O is dissolved into the HCl of 50ml
(0.01M) in, under agitation, it is added dropwise in 500ml NaOH (1.5M).Whole Deca building-up process keeps temperature
Spend for 80 DEG C and logical N2Except O2, the precipitation for being immediately generated black is reacted, the Fe that will be synthesized with Magnet3O4Nanoparticle is separated, and is used
100ml water washing 3 times, is dispersed in standby in five water of 500ml Tetramethylammonium hydroxide (0.1M)；
(2)Fe3O4The preparation of/Au, takes above-mentioned 75ml Fe3O4Nanoparticle dilutes 20 times, adds 75ml sodium citrate
(0.1M), stir 15 minutes under the rotating speed of 1000rpm, solution is heated to 80 DEG C, then is added dropwise over 7.5ml oxammonium hydrochloride.
(0.2M) gold chloride (HAuCl with the 1% of 6.3ml4), now, the color of solution becomes laking by black, continues at 80 DEG C
Continuous reaction 5-6 hour, the Fe that will be synthesized with Magnet3O4/ Au nanoparticle is separated, standby with 100ml water washing 3 times.
(3) preparation of golden magnetic ink, the 25% of total weight adds the Fe for preparing3O4/ Au powder body, 22.5% adds
Enter aqueous color paste, 55% adds polyurethane, and 20% adds ethanol, and 1% adds organic silicon defoamer, and 1% adds organosilicon moistening
Dispersant, 0.5% adds surfactant sodium dodecyl base benzenesulfonic acid；Add the Fe for accounting for water-based inks 25%3O4/ Au nanoparticle
Son is obtained final product.
Embodiment 2：
(1)Fe3O4The preparation of nanoparticle, by 8g FeCl3·6H2O and 5g FeCl2·4H2O is dissolved into the HCl of 60ml
(0.01M) in, under agitation, it is added dropwise in 600ml NaOH (1.5M), whole Deca building-up process keeps temperature
Spend for 80 DEG C and logical N2Except O2. reaction is immediately generated the precipitation of black, the Fe that will be synthesized with Magnet3O4Nanoparticle is separated, and is used
100ml water washing 3 times, is dispersed in standby in five water of 500ml Tetramethylammonium hydroxide (0.1M)；
(2)Fe3O4The preparation of/Au, takes above-mentioned 75ml Fe3O4Nanoparticle dilutes 20 times, adds 60ml sodium citrate
(0.15M), stir 15 minutes under the rotating speed of 1000rpm, solution is heated to 80 DEG C, then is added dropwise over 9ml oxammonium hydrochloride.
(0.2M) gold chloride (HAuCl with the 1% of 6.3ml4), now, the color of solution becomes laking by black, continues at 80 DEG C
Continuous reaction 5-6 hour, the Fe that will be synthesized with Magnet3O4/ Au nanoparticle is separated, standby with 100ml water washing 3 times.
(3) preparation of golden magnetic ink, according to the Fe that 25% addition of total weight is prepared3O4/ Au powder body,
26.5% adds aqueous color paste, and 55% adds polyurethane, and 15% adds ethanol, and 1% adds organic silicon defoamer, and 1% addition has
Machine silicon wetting dispersing agent, 1.5% adds surfactant sodium dodecyl base benzenesulfonic acid；Add the Fe for accounting for water-based inks 30%3O4/
Au nanoparticle is obtained final product.
Embodiment 3：
(1)Fe3O4The preparation of nanoparticle, by 9.6g FeCl3·6H2O and 4.5g FeCl2·4H2O is dissolved into the HCl of 55ml
(0.01M) in, under agitation, it is added dropwise in 500ml NaOH (1.5M), whole Deca building-up process keeps temperature
Spend for 80 DEG C and logical N2Except O2, the precipitation for being immediately generated black is reacted, the Fe that will be synthesized with Magnet3O4Nanoparticle is separated, and is used
100ml water washing 3 times, is dispersed in standby in five water of 500ml Tetramethylammonium hydroxide (0.1M)；
(2)Fe3O4The preparation of/Au, takes above-mentioned 85ml Fe3O4Nanoparticle dilutes 20 times, adds 85ml sodium citrate
(0.1M), stir 15 minutes under the rotating speed of 1000rpm, solution is heated to 80 DEG C, then is added dropwise over 9.5ml oxammonium hydrochloride.
(0.2M) gold chloride (HAuCl with the 1% of 6.3ml4), now the color of solution becomes laking by black, continues at 80 DEG C
Continuous reaction 5-6 hour.The Fe that will be synthesized with Magnet3O4/ Au nanoparticle is separated, standby with 100ml water washing 3 times.
(3) preparation of golden magnetic ink, 25% addition aqueous color paste, 55% addition polyurethane, 15% addition ethanol, 2%
Organic silicon defoamer is added, 2% adds organosilicon wetting dispersing agent, and 1% adds surfactant sodium dodecyl base benzenesulfonic acid, then presses
According to the Fe that 22% addition of total weight is prepared3O4/ Au powder body.
Water-based inks obtained by above-described embodiment are carried out with the detection that correlation prepares product, its result is as follows：
Nanometer gold Magnetic Characteristics of Magnetic Particles water-based inks obtained by embodiment as shown in Figure 1 are evenly distributed；
Nanoscale Fe3O4For permanent magnet, its magnetic will not be lost at normal temperatures, and because the Fe of mean diameter 16-100nm3O4
Routine (more than 100nm) Fe is above than remanence hardening strength and coercivity3O4Many, therefore in magnetic anti-counterfeit be all functionally
Conventional Fe3O4Cannot be comparable；
Profile be spherical or spherical be combined with ink by a certain percentage after both do not interfered with printing effect, turn avoid aciculiform
Magnetic iron oxide need to add the trouble of row's magnetic machine when using antiforge function；
Spheroidal for spherical or class 40nm or mean diameter are the Fe of 16-100nm3O4Powder body is mixed with ink according to a certain percentage
Magnetic ink is become after conjunction by four kilograms of spherical Fe3O4Powder body is put in the container equipped with high-boiling point alcohol, will with ultrasound wave
Aggregate in powder body scatter, after high temperature drying so that Fe3O4Again 10 kilograms of oil after formation lipophilic-hydrophobic property
Become stand-by magnetic by after ink and oleum lini are uniform after being mounted in being sufficiently stirred for of more than 40 minutes time of agitator tank central diameter together
Property ink.The viscosity (mPa s) for drawing after the test of digital rotating cylinder viscometer is 1043, and ink is coated at ambient temperature
On film, drying time is about 5-10min.
Magnetic Test is carried out to prepared sample, its step is as follows：Pretreatment process be fluid sample is mounted in closed
Certain specification container in, be then around primary coil and secondary coil.Apparatus measures, the magnetic field intensity that determined are used again
About 500-4500Gs.
It should be understood that these embodiments are only illustrative of the invention and is not intended to limit the scope of the invention.In addition, it is to be understood that
After the content for having read present invention instruction, those skilled in the art can be made various changes or modifications to the present invention, these
The equivalent form of value equally falls within the application appended claims limited range.
Claims (7)
1. a kind of nanometer gold Magnetic Characteristics of Magnetic Particles water-based inks, it is characterised in that by percentage by weight for the nanometer gold magnetic powder of 2-4% and
The water-based inks composition of 96%-98%.
2. a kind of nanometer gold Magnetic Characteristics of Magnetic Particles water-based inks, it is characterised in that described water-based inks include the water of 22.5-26.5%
Property mill base, the polyurethane of 55-60%, the ethanol of 15-20%, the surfactant of 2-5%.
3. the preparation method of a kind of nanometer gold Magnetic Characteristics of Magnetic Particles water-based inks according to claim 1, it is characterised in that described
Solvent be ethanol.
4. the preparation method of a kind of nanometer gold Magnetic Characteristics of Magnetic Particles water-based inks according to claim 1, it is characterised in that described
Surfactant be organic silicon defoamer, organosilicon wetting dispersing agent and DBSA.
5. the method for preparing a kind of nanometer gold Magnetic Characteristics of Magnetic Particles water-based inks in claim 1-4 described in any claim, its
It is characterised by, comprises the steps：
S1, preparation Fe3O4Nanoparticle：By FeCl3·6H2O and FeCl2·4H2O is dissolved in 0.01M HCl, in stirring condition
Under, it is added dropwise in NaOH, whole Deca building-up process keeping temperature is 60-80 DEG C, and leads to N2Except O2And keep 2-4 little
Shi Zhizhi generates the precipitation of black；
S2, take above-mentioned Fe3O4Nanoparticle dilutes 15-20 times, adds sodium citrate, stirs under the rotating speed of 1000-3000rpm
Mixing uniformly, solution is heated to 60-80 DEG C, then the gold chloride of 0.15-0.2M oxammonium hydrochloride. and 1-3% is added dropwise over to solution
Color becomes laking by black；
S3, at 60-80 DEG C continue reaction 5-6 hour, with Magnet will synthesize Fe3O4/ Au nanoparticle is separated, and uses distilled water
Standby after washing 2-3 time；
S4, in the Fe for preparing3O4In/Au powder body, addition aqueous color paste, solvent, surfactant and corresponding auxiliary agent are until raw
Become corresponding water-based inks.
6. a kind of preparation method of nanometer gold Magnetic Characteristics of Magnetic Particles water-based inks according to claim 1, it is characterised in that step
Lead to N in S12Except O2And 2-4 hour is kept until generating the precipitation of black.
7. a kind of preparation method of nanometer gold Magnetic Characteristics of Magnetic Particles water-based inks according to claim 1, it is characterised in that step
S1 prepares Fe3O4The Fe that will be synthesized with Magnet after nanoparticle3O4Nanoparticle is separated, and is washed with water 2-3 time, is disperseed
Standby in five water of Tetramethylammonium hydroxide.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610927232.0A CN106433289A (en) | 2016-10-31 | 2016-10-31 | Preparation method for magnetic water-based ink with nano-gold magnetic powder |
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| CN201610927232.0A CN106433289A (en) | 2016-10-31 | 2016-10-31 | Preparation method for magnetic water-based ink with nano-gold magnetic powder |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103602145A (en) * | 2013-10-26 | 2014-02-26 | 溧阳市东大技术转移中心有限公司 | Nanometer silver ink for printed circuit |
| CN104059430A (en) * | 2013-03-21 | 2014-09-24 | 中国科学院化学研究所 | Method for batch preparation of anisotropic particles by ink-jet printing and anisotropic particles thereof |
| CN104164136A (en) * | 2013-05-16 | 2014-11-26 | 中国科学院化学研究所 | Preparation method of petal-shaped anisotropic particle and petal-shaped anisotropic particle |
-
2016
- 2016-10-31 CN CN201610927232.0A patent/CN106433289A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104059430A (en) * | 2013-03-21 | 2014-09-24 | 中国科学院化学研究所 | Method for batch preparation of anisotropic particles by ink-jet printing and anisotropic particles thereof |
| CN104164136A (en) * | 2013-05-16 | 2014-11-26 | 中国科学院化学研究所 | Preparation method of petal-shaped anisotropic particle and petal-shaped anisotropic particle |
| CN103602145A (en) * | 2013-10-26 | 2014-02-26 | 溧阳市东大技术转移中心有限公司 | Nanometer silver ink for printed circuit |
Non-Patent Citations (1)
| Title |
|---|
| 葛兆强等: "Fe3O4@Au核壳纳米颗粒的制备及表征", 《热加工工艺》 * |
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