CN106566309A - Nanometer silver powder magnetic water-based ink and preparation method thereof - Google Patents
Nanometer silver powder magnetic water-based ink and preparation method thereof Download PDFInfo
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- CN106566309A CN106566309A CN201610927227.XA CN201610927227A CN106566309A CN 106566309 A CN106566309 A CN 106566309A CN 201610927227 A CN201610927227 A CN 201610927227A CN 106566309 A CN106566309 A CN 106566309A
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- water
- nanometer silver
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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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- 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
- C09D11/033—Printing inks characterised by features other than the chemical nature of the binder characterised by the solvent
-
- 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
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention relates to a nanometer silver powder magnetic water-based ink, which comprises, by weight, 2-4% of Fe3O4/Ag powder and 96-98% of water-based ink, wherein the water-based ink comprises 22.5-26.5% of an aqueous pigment paste, 55-60% of polyurethane, 15-20% of a solvent, and 2-5% of a surfactant. The preparation method specifically comprises: 1) preparing Fe3O4 nanoparticles; 2) preparing a Fe3O4/Ag complex; and 3) adding the Fe3O4 into a AgNO3 solution, carrying out ultrasonic treatment for half an hour, adding newly-prepared sodium hydroxide and hydroxylamine hydrochloride, mixing for 1 h, separating the synthesized Fe3O4/Ag nanoparticles by using a magnet, washing three times with 100 ml of ethanol. According to the present invention, the growth of bacteria in the ink can be inhibited with the addition of the Ag powder; with the application of the ethanol and the water as the solvent, the obtained ink is the environmentally friendly ink and has the low environmental pollution; the Ag/Fe3O4 is added in one time and has good dispersion property in the ink; and the prepared nanometer silver magnetic powder magnetic fluid has high magnetic induction strength and high stability.
Description
Technical field
The present invention relates to a kind of magnetic water-based inks, particularly a kind of nanometer silver Magnetic Characteristics of Magnetic Particles water-based inks.
Background technology
The false proof principle of magnetic ink is that color adopts magnetisable material, such as adds the chemicals such as cobalt in ferrum oxide or ferrum oxide
Matter, can detect that magnetic signal using Magnetic testi instrument and decodes.The characteristics of it projects is outward appearance color depth, and detecting instrument is simple, its skill
It is less than micron-sized acicular crystal, so that its size and shape is easily uniform in magnetic field arranging that art requirement is magnetic colorant
Row.
Magnetic printing product are the unique media for being combined with recording technique and printing technology and being produced, and are characterized in that data can be
Writing, reading on magnetic card, can visually see the magnetic printing basic fundamental of word, pattern and photo.As a kind of special
The anti-counterfeiting printing technology of ink is planted, it is all applied in many fields at present, for example ticket, monthly ticket, bank book, identity card
Deng.Magnetic ink constitutes identical with general ink substantially, i.e., be made up of pigment, binder, inserts and adjuvant.Magnetic ink institute
Pigment is not common colorant, but strong magnetic material.With the increase of magnetic ink usage amount, which is required also increasingly
Also there are many deficiencies in the magnetic ink on height, but market, heat resistance is not good, and adhesive force needs to improve.
Magnetic printing in order to prevent from forging and distort, to level security more and more higher, thus magnetic material, printing,
Special material or technology are adopted in processing method.With the progress of science and technology, the innovation of anti-counterfeiting technology and typography it is continuous
Improve, magnetic ink has played more and more important effect, and the utilization that combines with other anti-counterfeiting technologies in terms of anti-counterfeit printing
To all trades and professions.With use more and more extensively, to requirements also more and more higher, not only will its magnetic effect it is good, to magnetic powder
Require to be also big magnetic saturation, even particle size, good dispersion, stable, high so as to obtain comparison magnetic.
Fe of the unit particle diameter for 40nm3O4, its structure is changed into the Fe of single magnetic domain, i.e. single magnetic domain from many magnetic domains3O4To become
Permanent magnet, its magnetic property are never lost at normal temperatures, and because mean diameter is the Fe of 16nm-100nm3O4Ratio it is surplus
The residual magnetism intensity of magnetization and coercivity are above routine (more than 100nm) Fe3O4Many, therefore be functionally conventional in magnetic anti-counterfeit
Cannot be comparable.
The content of the invention
The invention discloses a kind of nanometer silver Magnetic Characteristics of Magnetic Particles water-based inks, with good printing and anti-counterfeiting performance.
A kind of nanometer silver Magnetic Characteristics of Magnetic Particles water-based inks, by the Fe that percentage by weight is 2-4%3O4/ Ag powder body and 96-98%
Water-based inks composition；Described water-based inks include the aqueous color paste of 22.5-26.5%, the polyurethane of 55-60%, 15-
20% solvent, the surfactant of 2-5%；Described solvent is ethanol；Described surfactant organic silicon type defoamer,
Organosilicon wetting dispersing agent and DBSA.
Nanometer silver Magnetic Characteristics of Magnetic Particles water-based inks are prepared, its step includes：
1) prepare Fe3O4Nanoparticle, by FeCl3·6H2O and FeCl2·4H2O is dissolved in HCl solution, is stirred at 60-90 DEG C
Mix, be added dropwise in NaOH solution, the Fe that will be synthesized with Magnet3O4Nanoparticle is separated, and removes surface with distilled water wash
It is standby after residual solution；
2) prepare Fe3O4/ Ag complex, Fe3O4Nanoparticle ultrasound 1-2 hours in ethanol, add 3- aminopropyl front threes
TMOS, stirs 10-12 hours with 1000-3000rpm；
3)) again by above-mentioned Fe3O4It is added to AgNO3In solution, ultrasonic 1-2 hours add freshly prepd sodium hydroxide and hydrochloric acid
Azanol, mixes 1-3 hours, the Fe that will be synthesized with Magnet3O4/ Ag nanoparticles are separated, with washing with alcohol 2-3 time.Step 2) middle use
The Fe that Magnet will synthesize3O4After nanoparticle is separated, with 100ml washing with alcohol 3 times；Step 1) in whole Deca building-up process protect
Temperature is held for 80 DEG C；Step 1) in the solution lead to N2Except O2。
A kind of nanometer silver Magnetic Characteristics of Magnetic Particles water-based inks of the present invention, contrast prior art have the advantage that：
(1) addition of Ag powder can suppress the growth of antibacterial in ink；
(2) second alcohol and water being used as solvent, being a kind of ink of environmental protection, environmental pollution is little；
(3)Ag/Fe3O4Disposable to add, in ink, dispersive property is good；
(4) the nanometer silver magnetic powder magnetic fluid prepared by, with higher magnetic induction and stability.
Description of the drawings
Fig. 1 is Fe3O4The TEM figures of/Ag nanoparticles.
Specific embodiment
Below by way of specific embodiment, the present invention is further elaborated, but not as a limitation of the invention.
Embodiment one
1)Fe3O4The preparation of nanoparticle
By 10.8g FeCl3·6H2O and 4.0g FeCl2·4H2O is dissolved in the HCl (0.01M) of 50ml, in stirring condition
Under, it is added dropwise in 500ml NaOH (1.5M), whole Deca building-up process keeping temperature is 80 DEG C and logical N2Except O2, instead
The precipitation of black should be immediately generated, the Fe that will be synthesized with Magnet3O4Nanoparticle is separated, with standby after 100ml water washings 3 times；
2)Fe3O4The preparation of/Ag
2.5g Fe3O4Nanoparticle is added to ultrasonic half an hour in 100mL ethanol, adds 10mL 3- aminopropyl trimethoxies
Base silane, is stirred 12 hours with 2000rpm.The Fe that will be synthesized with Magnet3O4Nanoparticle is separated, with 100ml washing with alcohol 3 times.
Again by 5g above-mentioned Fe3O4It is added to the AgNO of 1L 1.5wt.%3In solution, ultrasonic half an hour, freshly prepd 5L, 0.1M are added
Sodium hydroxide and 4.5L 0.06M oxammonium hydrochloride. in, mix 1 hour, with Magnet will synthesize Fe3O4/ Ag nanoparticles point
From with 100ml washing with alcohol 3 times；
3) preparation of silver-colored magnetic ink
According to 22.5% addition aqueous color paste of total weight, 55% adds polyurethane, and 17.5% adds ethanol, and 2% adds
Organic silicon type defoamer, 2% adds organosilicon wetting dispersing agent, and 1% adds surfactant sodium dodecyl base benzenesulfonic acid；Add
Account for 4% Fe3O4/ Ag powder body.
Embodiment two
1)Fe3O4The preparation of nanoparticle
By 8.8g FeCl3·6H2O and 4.0g FeCl2·4H2O is dissolved in the HCl (0.01M) of 50ml, under agitation,
It is added dropwise in 500ml NaOH (1.5M), whole Deca building-up process keeping temperature is 80 DEG C and logical N2Except O2, react vertical
The precipitation of black, the Fe that will be synthesized with Magnet are generated3O4Nanoparticle is separated, with 100ml water washings 3 times；
2)Fe3O4The preparation of/Ag
3.5g Fe3O4Nanoparticle is added to ultrasonic half an hour in 100mL ethanol, adds 8mL 3- aminopropyl trimethoxies
Base silane, is stirred 12 hours with 2000rpm.The Fe that will be synthesized with Magnet3O4Nanoparticle is separated, with 100ml washing with alcohol 3 times.
Again by 5.5g above-mentioned Fe3O4It is added to the AgNO of 1L 1.5wt.%3In solution, ultrasonic half an hour, freshly prepd 5L is added,
In the oxammonium hydrochloride. of the sodium hydroxide and 4.5L0.06M of 0.1M, mix 1 hour, the Fe that will be synthesized with Magnet3O4/ Ag nanoparticles
Separate, with 100ml washing with alcohol 3 times；
3) preparation of silver-colored magnetic ink
Water-based inks are prepared first, its component adds aqueous color paste according to 26.5%, 65% adds polyurethane, and 17.5% adds second
Alcohol, 1% adds organic silicon type defoamer；Add the Fe for accounting for 2%3O4/ Ag powder body.
Embodiment three
1)Fe3O4The preparation of nanoparticle
By 7.5g FeCl3·6H2O and 5.0g FeCl2·4H2O is dissolved in the HCl (0.01M) of 50ml, under agitation,
It is added dropwise in 500ml NaOH (1.5M).Whole Deca building-up process keeping temperature is 80 DEG C and logical N2Except O2, react vertical
The precipitation of black is generated.The Fe that will be synthesized with Magnet3O4Nanoparticle is separated, with 100ml water washings 3 times, standby；
2)Fe3O4The preparation of/Ag
3.5g Fe3O4Nanoparticle is added to ultrasonic half an hour in 100mL ethanol, adds 15mL 3- aminopropyl trimethoxies
Base silane, is stirred 12 hours with 2000rpm.The Fe that will be synthesized with Magnet3O4Nanoparticle is separated, with 100ml washing with alcohol 3 times.
Again by 8g above-mentioned Fe3O4It is added to the AgNO of 1.2L 1.5wt.%3In solution, ultrasonic half an hour, freshly prepd 5L is added,
In the oxammonium hydrochloride. of the sodium hydroxide and 5.5L0.06M of 0.1M, mix 1 hour, the Fe that will be synthesized with Magnet3O4/ Ag nanoparticles
Separate, with 100ml washing with alcohol 3 times；
3) preparation of silver-colored magnetic ink
Water-based inks are prepared first, successively 23.5% addition aqueous color paste, 55% addition polyurethane, 17.5% addition ethanol, 1%
Organic silicon type defoamer is added, 1% adds organosilicon wetting dispersing agent, and 2% adds surfactant sodium dodecyl base benzenesulfonic acid；Again
Addition accounts for 3% Fe3O4/ Ag powder body.
Magnetic ink has the drawback that oil absorption than larger, and transfer performance is nor feel quite pleased, therefore some are granular
Or cubical iron oxides, to improve its printing performance, as the residual magnetic of these iron oxides is poor, therefore consumption is not
Preferably excessive, for different printing processes, the particle diameter of the Magnaglo of selection may be different, but whatsoever printing process, magnetic
Property ink in magnetic paint characteristic be substantially the same, different mainly binders, it is also possible in being exactly ink formulations
The difference of composition proportion.
Nano-Ag particles as shown in Figure 1, in 30-40nm or so, its even particle distribution, size are homogeneous for its size；Jing
Test shows that the magnetic induction of magnetic ink magnetic fluid of the present invention is that solid content is in 30- between 500-4200Gs
Between 60%, have the advantages that magnetic force is strong, thus with good printing performance, in addition, Ag is a kind of anti-biotic material, can press down
The growth of antibacterial in liquefaction ink.It is 1043 digital rotating cylinder viscometer to be carried out to which and tests the viscosity (mPas) that can be drawn, ink
It is coated on film at ambient temperature, drying time is about 5-10min.
Certainly, the above is only the concrete application example of the present invention, protection scope of the present invention is not limited in any way, is removed
Outside above-described embodiment, the present invention can also have the technical side that other embodiment, all employing equivalents or equivalent transformation are formed
Case, all falls within scope of the present invention.
Claims (8)
1. a kind of nanometer silver Magnetic Characteristics of Magnetic Particles water-based inks, it is characterised in that by percentage by weight for 2-4% Fe3O4/ Ag powder body
Constitute with the water-based inks of 96-98%.
2. a kind of nanometer silver 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 solvent of 15-20%, the surfactant of 2-5%.
3. a kind of nanometer silver Magnetic Characteristics of Magnetic Particles water-based inks according to claim 1, it is characterised in that described solvent is second
Alcohol.
4. a kind of nanometer silver Magnetic Characteristics of Magnetic Particles water-based inks according to claim 1, it is characterised in that described surface activity
Agent is organic silicon defoamer, organosilicon wetting dispersing agent and DBSA.
5. a kind of nanometer silver Magnetic Characteristics of Magnetic Particles water-based inks described in any claim in claim 1-4 are prepared, and its feature exists
In concrete steps include：
1) prepare Fe3O4Nanoparticle, by FeCl3·6H2O and FeCl2·4H2O is dissolved in HCl solution, is stirred at 60-90 DEG C
Mix, be added dropwise in NaOH solution, the Fe that will be synthesized with Magnet3O4Nanoparticle is separated, and removes surface with distilled water wash
It is standby after residual solution；
2) prepare Fe3O4/ Ag complex, Fe3O4Nanoparticle ultrasound 1-2 hours in ethanol, add 3- aminopropyl front threes
TMOS, stirs 10-12 hours with 1000-3000rpm；
3) again by above-mentioned Fe3O4It is added to AgNO3In solution, ultrasonic 1-2 hours add freshly prepd sodium hydroxide and hydrochloric acid
Azanol, mixes 1-3 hours, the Fe that will be synthesized with Magnet3O4/ Ag nanoparticles are separated, with washing with alcohol 2-3 time.
6. a kind of preparation method of nanometer silver Magnetic Characteristics of Magnetic Particles water-based inks according to claim 2, it is characterised in that：Step 2)
The middle Fe that will be synthesized with Magnet3O4After nanoparticle is separated, with washing with alcohol 2-3 time.
7. a kind of preparation method of nanometer silver Magnetic Characteristics of Magnetic Particles water-based inks according to claim 5, it is characterised in that：Step 1)
In whole Deca building-up process keeping temperature be 80 DEG C.
8. a kind of preparation method of nanometer silver Magnetic Characteristics of Magnetic Particles water-based inks according to claim 5, it is characterised in that：Step 1)
In in the solution lead to N2Except O2。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610927227.XA CN106566309A (en) | 2016-10-31 | 2016-10-31 | Nanometer silver powder magnetic water-based ink and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610927227.XA CN106566309A (en) | 2016-10-31 | 2016-10-31 | Nanometer silver powder magnetic water-based ink and preparation method thereof |
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| CN106566309A true CN106566309A (en) | 2017-04-19 |
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| CN201610927227.XA Pending CN106566309A (en) | 2016-10-31 | 2016-10-31 | Nanometer silver powder magnetic water-based ink and preparation method thereof |
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Citations (2)
| 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 |
| CN105936769A (en) * | 2016-05-25 | 2016-09-14 | 青岛瑞利特新材料科技有限公司 | Graphene modified nano-silver aqueous conductive ink and preparation method thereof |
-
2016
- 2016-10-31 CN CN201610927227.XA patent/CN106566309A/en active Pending
Patent Citations (2)
| 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 |
| CN105936769A (en) * | 2016-05-25 | 2016-09-14 | 青岛瑞利特新材料科技有限公司 | Graphene modified nano-silver aqueous conductive ink and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| JINGJING DU ET.CL: "preparation of Fe3O4@Ag SERS substrate and its application in environmental Cr(VI) analysis", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》 * |
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Application publication date: 20170419 |