CN102766357A - Method for preparing magnetic permeability pearlescent pigment - Google Patents
Method for preparing magnetic permeability pearlescent pigment Download PDFInfo
- Publication number
- CN102766357A CN102766357A CN2012102837632A CN201210283763A CN102766357A CN 102766357 A CN102766357 A CN 102766357A CN 2012102837632 A CN2012102837632 A CN 2012102837632A CN 201210283763 A CN201210283763 A CN 201210283763A CN 102766357 A CN102766357 A CN 102766357A
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- CN
- China
- Prior art keywords
- pearlescent pigment
- filter cake
- magnetic permeability
- preparation
- magnetic conductive
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000000049 pigment Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title abstract description 6
- 230000035699 permeability Effects 0.000 title abstract 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012065 filter cake Substances 0.000 claims abstract description 11
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 7
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- 229960002089 ferrous chloride Drugs 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims abstract description 6
- 239000000047 product Substances 0.000 claims abstract description 5
- 238000000967 suction filtration Methods 0.000 claims abstract description 4
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims description 16
- 239000011324 bead Substances 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 229960001866 silicon dioxide Drugs 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 230000000007 visual effect Effects 0.000 abstract description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 abstract 2
- 238000005406 washing Methods 0.000 abstract 2
- 238000001816 cooling Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 239000011049 pearl Substances 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 20
- 239000000243 solution Substances 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 229910018125 Al-Si Inorganic materials 0.000 description 3
- 229910018520 Al—Si Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- UCNNJGDEJXIUCC-UHFFFAOYSA-L hydroxy(oxo)iron;iron Chemical compound [Fe].O[Fe]=O.O[Fe]=O UCNNJGDEJXIUCC-UHFFFAOYSA-L 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052743 krypton Inorganic materials 0.000 description 1
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229910052704 radon Inorganic materials 0.000 description 1
- SYUHGPGVQRZVTB-UHFFFAOYSA-N radon atom Chemical compound [Rn] SYUHGPGVQRZVTB-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Hard Magnetic Materials (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention relates to a method for preparing a magnetic permeability pearlescent pigment. The method is characterized by including the following steps of firstly, adding a pearlescent pigment into water and heating the water to 80DEG C; secondly, adding a ferrous chloride solution under the atmosphere of inert gases and adjusting potential of hydrogen (pH) value to 6; thirdly, dropwise adding a potassium chlorate solution and cooling after a reaction; fourthly, performing a vacuum filtration, washing a filter cake by deionized water, adding the filter cake into water again, and heating the water to 80DEG C; fifthly, dropwise adding a sodium silicate solution and an aluminum chloride solution, stirring, adjusting the pH value to 7, performing a suction filtration after a reaction, and washing the filter cake by the deionized water; and sixthly, drying the filter cake at the temperature of 105 DEG C, and calcining the filter cake at the atmosphere of the inert gases to obtain a finished product. Compared with methods for preparing the magnetic permeability pearlescent pigment in prior art, the method has the advantages that the magnetic permeability pearlescent pigment has a high magnetic characteristic and attractive gloss like pearls, when magnetic permeability pearlescent pigment is sprayed or printed and is not dried, the magnetic permeability pearlescent pigment has an entertaining magnetic traveling phenomenon under a certain magnetic field action, and thereby a three-dimensional visual effect can be generated.
Description
Technical field
The present invention relates to a kind of preparation method of magnetic conductive bead delustering pigment, belong to ornamental pigment prepared field.
Background technology
Publication number is in the 101445674A China description of the invention, discloses a kind of magnetic pearlescent pigment and preparation method thereof.This preparation method is through the Fe of configuration certain mol proportion
3+And Fe
2+Solution, put into substrate, make Fe through regulating pH value then
3O
4Be coated on substrate surface.This preparation method needs accurately control PH, and the control difficulty is big; And this preparation method needs accurately preparation Fe
3+And Fe
2+Ratio, the preparation difficulty higher.
Summary of the invention
The objective of the invention is to overcome the above-mentioned deficiency that exists in the prior art, and provide a kind of step few, control is simple, the preparation method of the magnetic conductive bead delustering pigment of inexpensive.
The present invention addresses the above problem the technical scheme that is adopted: the preparation method of this magnetic conductive bead delustering pigment is characterized in that may further comprise the steps.
A) pearly pigment is added in the entry, and be warming up to 80 ℃.The compactness and the intensity of the Z 250 that this temperature can guarantee to coat.
B) under inert gas atmosphere, add solution of ferrous chloride, and regulate PH to 6.The solution of ferrous chloride low price.
C) drip the potassium chlorate solution, question response finishes postcooling.Drip the potassium chlorate solution, control easily, iron protochloride oxidation extremely easily, speed of response is fast, and the reaction times is short, makes that control is convenient.
D) vacuum filtration is also used the deionized water flush cake, filter cake is added in the entry again, and be heated to 80 ℃.Remove the unnecessary material in surface, guarantee the final cost quality.
E) drip sodium silicate solution and liquor alumini chloridi, stir and regulate PH to 7, question response finishes the back suction filtration and uses the deionized water flush cake.Form the Al-Si composite package, play a protective role, can improve weathering resistance.This Al-Si composite package is coated on Fe
3O
4Outside the film, has protection Fe
3O
4The function of film.Al-Si composite package intensity is high, and hardness is big, can effectively prevent to scratch Fe
3O
4Film.
F) filter cake is dried down in 105 ℃, calcining under inert gas atmosphere then obtains finished product.
The potassium chlorate solution's concentration that drips among the step c of the present invention is 300g/L.
Calcining temperature is 560 ℃ among the step f of the present invention, and calcination time is 30 minutes.
Rare gas element of the present invention is a nitrogen.
The sodium silicate solution that step e of the present invention drips and the concentration of liquor alumini chloridi are respectively: in silicon-dioxide, and mass content 10%; With AlCl
3Meter, mass content 10%.
The present invention compared with prior art; Have the following advantages and effect: the magnetic conductive bead delustering pigment has stronger magnetic characteristic; It not only has charming gloss as the pearl; And under certain the action of a magnetic field, can demonstrate the very witty magnetic phenomenon of walking when not dried, thereby the visual effect of generation 3 D stereo in spraying or printing.
Iron black Chemical Composition is a Z 250, has ferromagnetism, is that magnetic is the strongest in the mineral, can be by permanent magnet attraction.The present invention utilizes this characteristic of Z 250 exactly, with the pearly pigment be base material at its coated with uniform one deck nano level Z 250, thereby make pigment have magnetic characteristic.The present invention is a raw material with the iron protochloride that is prone to obtain, and is oxygenant with Potcrate, selects for use oxidation-precipitation method to make Z 250.
Its reaction principle is following:
FeCl
2+2NaOH=Fe(OH)
2↓+2NaCl (Ⅰ)
2KClO
3 Heating2KCl+O
2↑ (II)
4Fe(OH)
2+O
2+2H
2O=4Fe(OH)
3↓ (Ⅲ)
Fe (OH)
2+ 2Fe (OH)
3=FeOFe
20
34H
2O
DehydrationFe
30
4+ 4H
20 (IV)
In the aqueous solution that is added with pearly pigment (80 ℃), add solution of ferrous chloride having under the situation of nitrogen protection, adding an amount of sodium hydroxide simultaneously, to be neutralized to PH about 6, makes part Fe
2+Form darkcyan or green Fe (OH)
2↓, add the potassium chlorate solution then, keep PH5-6, let part Fe
2+Be oxidized to Fe
3+, Fe (OH)
2And Fe (OH)
3Produce the nanometer Fe that coprecipitation reaction generates black by the formula IV
30
4, be coated on the pearly pigment surface by the Van der Waals force even action.For temperature tolerance and the resistance to corrosion that improves pigment, coat layer of aluminum silicon composite package again in surface of pigments.
Embodiment
The present invention is described in further detail below by embodiment, and following examples are to explanation of the present invention and the present invention is not limited to following examples.
Embodiment 1.
The preparation method of the magnetic conductive bead delustering pigment in the present embodiment may further comprise the steps.
A) be that pearly pigment and the suitable quantity of water of FWD120 poured in the 1000ml there-necked flask with the 50g model, add water to 600ml scale position, stir then and make pearly pigment make its homodisperse, be warming up to 80 ℃, keep this temperature.
B) in there-necked flask, charge into nitrogen with 0.2L/ minute speed, the air in the displacement there-necked flask.Under nitrogen atmosphere, adding 20mL concentration is the solution of ferrous chloride of 300g/L then, and adds sodium hydroxide solution adjusting PH to 6.
C) dripping 23.6mL concentration is the 30g/L potassium chlorate solution, and Potcrate is Fe partly
2+Be oxidized to Fe
3+, question response finishes postcooling.
D) vacuum filtration is also used the deionized water flush cake, filter cake is dropped into again add water to the 700mL liquid level in the 1000mL beaker, stirs, and transfers and is warming up to 80 ℃.
E) slowly drip 165mL sodium silicate solution and 27.5mL liquor alumini chloridi, stir and keep and regulate PH to 7 with 5% hydrochloric acid, stir half a hour after, suction filtration is also with deionized water flush cake 6 times.
F) filter cake among the step e is drained the back in 105 ℃ of oven dry down, under nitrogen atmosphere, calcined 30 minutes down then, obtain finished product in 560 ℃.
Among the present invention, the concentration of the sodium silicate solution among the step e is: in silicon-dioxide, and mass content 10%.
Among the present invention, the concentration of the liquor alumini chloridi among the step e is: with AlCl
3Meter, mass content 10%.
Among the present invention, the concentration of hydrochloric acid among the step e is: mass content 5%.
Among the present invention, rare gas element is meant the inactive gases of chemical property such as nitrogen, helium, neon, argon gas, krypton gas, xenon and radon gas.
Among the present invention, the liquor alumini chloridi among the step e is to use AlCl
36H
2O and zero(ppm) water are formulated.
Among the present invention, the clad ratio of Z 250 is 5-22%.
Among the present invention, the particle diameter of finished product magnetic conductive bead delustering pigment is the 5-250 micron.
Above content described in this specification sheets only is illustrating that the present invention is done.Person of ordinary skill in the field of the present invention can make various modifications or replenishes or adopt similar mode to substitute described specific embodiment; Only otherwise depart from the content of specification sheets of the present invention or surmount the defined scope of these claims, all should belong to protection scope of the present invention.
Claims (5)
1. the preparation method of a magnetic conductive bead delustering pigment is characterized in that may further comprise the steps:
A) pearly pigment is added in the entry, and be warming up to 80 ℃;
B) under inert gas atmosphere, add solution of ferrous chloride, and regulate PH to 6;
C) drip the potassium chlorate solution, question response finishes postcooling;
D) vacuum filtration is also used the deionized water flush cake, filter cake is added in the entry again, and be heated to 80 ℃;
E) drip sodium silicate solution and liquor alumini chloridi, stir and regulate PH to 7, question response finishes the back suction filtration and uses the deionized water flush cake;
F) filter cake is dried down in 105 ℃, calcining under inert gas atmosphere then obtains finished product.
2. the preparation method of magnetic conductive bead delustering pigment according to claim 1 is characterized in that: the potassium chlorate solution's concentration that drips among the step c is 300g/L.
3. the preparation method of magnetic conductive bead delustering pigment according to claim 1 and 2 is characterized in that: calcining temperature is 560 ℃ among the step f, and calcination time is 30 minutes.
4. the preparation method of magnetic conductive bead delustering pigment according to claim 1 and 2 is characterized in that: described rare gas element is a nitrogen.
5. the preparation method of magnetic conductive bead delustering pigment according to claim 1 and 2 is characterized in that: the sodium silicate solution that step e drips and the concentration of liquor alumini chloridi are respectively: in silicon-dioxide, and mass content 10%; With AlCl
3Meter, mass content 10%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102837632A CN102766357A (en) | 2012-08-10 | 2012-08-10 | Method for preparing magnetic permeability pearlescent pigment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102837632A CN102766357A (en) | 2012-08-10 | 2012-08-10 | Method for preparing magnetic permeability pearlescent pigment |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102766357A true CN102766357A (en) | 2012-11-07 |
Family
ID=47093953
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012102837632A Pending CN102766357A (en) | 2012-08-10 | 2012-08-10 | Method for preparing magnetic permeability pearlescent pigment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102766357A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103602102A (en) * | 2013-11-15 | 2014-02-26 | 浙江凯色丽科技发展有限公司 | 3D (Three-Dimensional) color-changing shimmer pigment |
| CN103694746A (en) * | 2013-12-27 | 2014-04-02 | 广东维诺珠光颜料有限公司 | Preparation method of multifunctional magnetic synthetic mica pearlescent pigment |
| CN104149485A (en) * | 2014-04-18 | 2014-11-19 | 上海紫江喷铝环保材料有限公司 | Device and method for transferring 3D pearly luster effect pattern |
| CN104893366A (en) * | 2015-06-18 | 2015-09-09 | 广西七色珠光材料股份有限公司 | Magnetic pearlescent pigment with 3D (three-dimensional) effect and preparation method of magnetic pearlescent pigment |
| CN106433287A (en) * | 2016-09-24 | 2017-02-22 | 德信嘉邦涂料（深圳）有限公司 | Application of magnetic ink in label |
| CN106752653A (en) * | 2015-11-19 | 2017-05-31 | 浙江伟星实业发展股份有限公司 | A kind of pearly-lustre button and preparation method thereof |
| CN110713736A (en) * | 2019-10-31 | 2020-01-21 | 南阳市凌宝珠光颜料有限公司 | Preparation method of color magnetic bead optical pigment |
| CN113527914A (en) * | 2021-07-22 | 2021-10-22 | 浙江瑞成新材料股份有限公司 | Magnetic pearlescent pigment and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103602102A (en) * | 2013-11-15 | 2014-02-26 | 浙江凯色丽科技发展有限公司 | 3D (Three-Dimensional) color-changing shimmer pigment |
| CN103694746A (en) * | 2013-12-27 | 2014-04-02 | 广东维诺珠光颜料有限公司 | Preparation method of multifunctional magnetic synthetic mica pearlescent pigment |
| CN103694746B (en) * | 2013-12-27 | 2015-11-18 | 广东维诺珠光颜料有限公司 | A kind of preparation method of multifunctional magnetic synthetic mica pearlescent pigment |
| CN104149485A (en) * | 2014-04-18 | 2014-11-19 | 上海紫江喷铝环保材料有限公司 | Device and method for transferring 3D pearly luster effect pattern |
| CN104149485B (en) * | 2014-04-18 | 2016-03-16 | 上海紫江喷铝环保材料有限公司 | The transfer device of the three-dimensional pearl effect pattern of a kind of 3D and transfer method |
| CN104893366A (en) * | 2015-06-18 | 2015-09-09 | 广西七色珠光材料股份有限公司 | Magnetic pearlescent pigment with 3D (three-dimensional) effect and preparation method of magnetic pearlescent pigment |
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Application publication date: 20121107 |