CN102766357A - Method for preparing magnetic permeability pearlescent pigment - Google Patents

Method for preparing magnetic permeability pearlescent pigment Download PDF

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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
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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.)
Pending
Application number
CN2012102837632A
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Chinese (zh)
Inventor
严文洲
蒋汉文
沈艳娥
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HANGZHOU FORWARD FINE CHEMICALS Co Ltd
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HANGZHOU FORWARD FINE CHEMICALS Co Ltd
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Application filed by HANGZHOU FORWARD FINE CHEMICALS Co Ltd filed Critical HANGZHOU FORWARD FINE CHEMICALS Co Ltd
Priority to CN2012102837632A priority Critical patent/CN102766357A/en
Publication of CN102766357A publication Critical patent/CN102766357A/en
Pending legal-status Critical Current

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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

A kind of preparation method of magnetic conductive bead delustering pigment
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%.
CN2012102837632A 2012-08-10 2012-08-10 Method for preparing magnetic permeability pearlescent pigment Pending CN102766357A (en)

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Cited By (8)

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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)

* Cited by examiner, † Cited by third party
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
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
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
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
CN113527914B (en) * 2021-07-22 2022-05-27 浙江瑞成新材料股份有限公司 Magnetic pearlescent pigment and preparation method thereof

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Application publication date: 20121107