CN113527914B - Magnetic pearlescent pigment and preparation method thereof - Google Patents

Magnetic pearlescent pigment and preparation method thereof Download PDF

Info

Publication number
CN113527914B
CN113527914B CN202110830795.9A CN202110830795A CN113527914B CN 113527914 B CN113527914 B CN 113527914B CN 202110830795 A CN202110830795 A CN 202110830795A CN 113527914 B CN113527914 B CN 113527914B
Authority
CN
China
Prior art keywords
magnetic
pearlescent pigment
powder
magnetic powder
weight
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.)
Active
Application number
CN202110830795.9A
Other languages
Chinese (zh)
Other versions
CN113527914A (en
Inventor
柳继成
穆彬
张海滨
郭永城
龚昌港
霍海元
李善云
温正助
郑洁
孔令利
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhejiang Ruicheng New Materials Co ltd
Original Assignee
Zhejiang Ruicheng New Materials Co ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Zhejiang Ruicheng New Materials Co ltd filed Critical Zhejiang Ruicheng New Materials Co ltd
Priority to CN202110830795.9A priority Critical patent/CN113527914B/en
Publication of CN113527914A publication Critical patent/CN113527914A/en
Application granted granted Critical
Publication of CN113527914B publication Critical patent/CN113527914B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0015Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds
    • C09C3/063Coating
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/42Magnetic properties
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C2200/00Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/40Interference pigments comprising an outermost surface coating
    • C09C2200/401Inorganic protective coating
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C2220/00Methods of preparing the interference pigments
    • C09C2220/10Wet methods, e.g. co-precipitation

Abstract

The invention discloses a magnetic pearlescent pigment and a preparation method thereof, wherein the magnetic pearlescent pigment comprises a pearlescent pigment and a magnetic powder coating layer arranged on the surface of the pearlescent pigment, the magnetic powder coating layer is a silicon dioxide layer dispersed with magnetic powder, and the magnetic powder is magnetic nano iron powder. The invention adopts the nanometer iron powder with high saturation magnetization as the magnetic source, and the metal simple substance iron is coated on the surface of the common pearlescent pigment, thereby greatly breaking through the magnetic strength of the current magnetic pearlescent pigment.

Description

Magnetic pearlescent pigment and preparation method thereof
Technical Field
The invention belongs to the technical field of decoration, and particularly relates to a magnetic pearlescent pigment and a preparation method thereof.
Background
The pearlescent pigment is a special pigment prepared by coating metal oxides with different refractive indexes on the surface of a flaky substrate such as mica, glass and the like, and common metal oxide layers comprise titanium dioxide, iron oxide, silicon dioxide and the like. The incident light generates interference phenomenon at the interface of the coating layer and the substrate layer of the pearlescent pigment, thereby generating interference color. Pearlescent pigments are widely used in the fields of paints, plastics, inks, cosmetics, etc., and impart a sense of high-priced, profound, and spacious to the decorated products, thereby improving the added value of the products. Along with the development of social economy and the remarkable improvement of living standard of people, along with the promotion and the aging of decoration, the pearlescent pigment with additional functions is produced.
The 3D magnetic pearlescent pigment as a high-grade pearlescent pigment becomes a new favorite for fashion and decoration. After the paint, nail polish or ink containing the magnetic pearlescent pigment is constructed on the surface of an object, magnets with beautiful patterns are placed below the paint, nail polish or ink, the flaky magnetic pearlescent pigment is arranged according to the shape of the magnets, and a unique 3D stereoscopic effect and fantastic brilliant colors can be formed after the flaky magnetic pearlescent pigment is solidified. The coating is widely applied to various fields such as 3D glass paint, artificial leather, cat eye nail polish, wallpaper coating and the like, and is popular with people.
The magnetic pearlescent pigment product on the market at present is prepared by coating a layer of magnetic material on the surface of common pearlescent pigment, mainly ferroferric oxide, cobalt oxide or a mixture thereof. Patent CN101445674B hydrolyzes ferric iron and ferrous iron salt solution at a certain pH value, deposits ferroferric oxide on a flaky substrate, and calcines in inert atmosphere to obtain the magnetic pearlescent pigment. The ferroferric oxide prepared by the method is directly exposed on the surface of the flaky substrate, is easy to be oxidized and lose magnetism, is not easy to be stored for a long time, and the inert atmosphere calcination has higher requirements on large-scale industrialized calcination equipment. Patent CN102766357A proposes a method for preparing magnetic pearlescent pigment, in which potassium chlorate solution is dropped into mixed solution containing ferrous chloride solution and common pearlescent pigment under inert atmosphere, ferroferric oxide is deposited on the common pearlescent pigment, then a protective layer of silicon dioxide and aluminum oxide is coated, and the magnetic pearlescent pigment is obtained after calcination under inert atmosphere condition. Patent CN104893366B discloses a magnetic pearlescent pigment with 3D effect, in which the surface of a common pearlescent pigment is coated with a magnetic layer of cobalt oxide, iron oxide and ferrous oxide, and then coated with a protective layer of silicon dioxide and aluminum oxide. This process also requires high-temperature calcination and the presence of cobalt also limits its use in the cosmetic field.
The invention patents all utilize the magnetism of iron or cobalt oxide to prepare the magnetic pearlescent pigment, and the magnetic source is single and the magnetic strength is weaker. Therefore, the development and preparation of the magnetic pearlescent pigment with different magnetic sources and better magnetic strength have positive significance.
Disclosure of Invention
The invention aims to provide a magnetic pearlescent pigment and a preparation method thereof, which can overcome the defects in the background art.
Therefore, the invention adopts the following technical proposal,
the magnetic pearlescent pigment comprises pearlescent pigment and a magnetic powder coating layer arranged on the surface of the pearlescent pigment, wherein the magnetic powder coating layer is a silicon dioxide layer dispersed with magnetic powder, and the magnetic powder is magnetic nano iron powder.
Optionally, the pearlescent pigment is prepared by coating mica or glass or silica or alumina flaky substrate with metal oxides with different refractive indexes.
Optionally, the pearlescent pigment is composed of mica or glass or silica or alumina flaky substrates coated with titanium dioxide, or mica or glass or silica or alumina flaky substrates coated with titanium dioxide and ferric oxide, or mica or glass or silica or alumina flaky substrates coated with ferric oxide.
Preferably, the particle size of the pearlescent pigment is 5-1000 μm; more preferably, the pearlescent pigment has a particle size of 5 to 25 μm or 10 to 60 μm or 20 to 100 μm, the smaller the particle size, the more silky, the more glittering effect is exhibited after the pigment is applied, and the user can select the desired effect.
The invention also provides a preparation method of the magnetic pearlescent pigment, which comprises the following steps:
coating a silicon dioxide layer containing magnetic powder on the surface of the pearlescent pigment, wherein the magnetic powder is magnetic nano iron powder;
the silicon dioxide layer containing the magnetic powder is prepared by a sol-gel method without high-temperature calcination, and the coating process comprises the following steps:
s1, grinding and dispersing the magnetic powder raw material, tetraethyl orthosilicate and a silane coupling agent together to obtain magnetic powder with the surface grafted with the silane coupling agent, wherein the grafted magnetic powder is uniformly and stably dispersed in the tetraethyl orthosilicate;
s2, mixing the pearlescent pigment and the alcohol organic solvent, adding an alkaline catalyst, stirring and heating, adding the tetraethyl orthosilicate solution which is obtained in the step S1 and is uniformly and stably dispersed with the grafted magnetic powder, reacting together, filtering, washing and drying to obtain the pearlescent pigment.
Preferably, in the coating process, the addition amounts of the pearlescent pigment, the magnetic powder raw material and the tetraethyl orthosilicate are as follows according to parts by weight: 100 parts by weight, 2-10 parts by weight and 20-100 parts by weight.
Preferably, in step S1, the magnetic powder raw material is magnetic nano iron powder with a particle size of 10-50 nm.
Optionally, in step S2, the alcohol is one or more of ethanol, butanol, and isopropanol.
Optionally, in step S2, the basic catalyst is aqueous ammonia, or aqueous solution of ethylenediamine, or triethylamine, or tributylamine, and the temperature is raised to 65-80 ℃ by stirring, wherein the reaction time of the co-reaction is 2-6 hours.
Optionally, the addition amount of the silane coupling agent is 0.2% -1% of the weight of the magnetic nano iron powder.
Compared with the background technology, the technical scheme at least has the following advantages:
1. the magnetic pearlescent pigment provided by the invention comprises a pearlescent pigment and a magnetic powder coating layer arranged on the surface of the pearlescent pigment, wherein the magnetic powder coating layer is a silicon dioxide layer dispersed with magnetic powder, and the magnetic powder is magnetic nano iron powder; according to the saturation magnetization data of a common magnetic material, under the normal temperature condition, the saturation magnetization of iron or cobalt oxide is 70-90emu/g, and the saturation magnetization of metallic elementary iron is 218emu/g which is far larger than that of the iron or cobalt oxide.
2. The magnetic powder coating layer is prepared by a sol-gel method without high-temperature calcination, and due to the principle of the sol-gel method, when orthosilicic acid is subjected to polymerization reaction, water molecules are removed and polymerized into a network structure of silicon dioxide, and after the coating is finished, the product does not need high-temperature calcination and dehydration, so that the chance of weakening the high-temperature magnetism of nano iron is reduced, the investment of high-temperature equipment is reduced, and the energy consumption is saved;
3. in the magnetic pearlescent pigment provided by the invention, the magnetic powder is dispersed in the silicon dioxide layer, and the silicon dioxide not only plays a role of adhering the nanometer iron powder on the surface of the pearlescent pigment, but also provides a protective layer for isolating air for the nanometer iron powder;
4. according to the preparation method of the magnetic pearlescent pigment, the silane coupling agent is adopted to treat the nano iron powder, so that the silane coupling agent is grafted on the surface of the nano iron powder and can be stably dispersed in tetraethyl orthosilicate; during reaction hydrolysis, silane groups on the surface of the nano iron powder and tetraethyl orthosilicate are hydrolyzed into orthosilicic acid, and then nano iron particles and silicon dioxide are deposited on the surface of the traditional pearlescent pigment together.
Drawings
FIG. 1 is a schematic structural diagram of a magnetic pearlescent pigment provided by the present invention;
fig. 2 is a reference diagram of a magnetic test experiment of the magnetic pearlescent pigment provided by the invention.
Detailed Description
The technical problems of single magnetic raw material and weaker magnetism of the magnetic pearlescent pigment in the prior art exist.
Therefore, the invention provides a novel magnetic pearlescent pigment and a preparation method thereof, so as to solve the technical problems.
Referring to fig. 1, the magnetic pearlescent pigment comprises a pearlescent pigment 100 and a magnetic powder coating layer 200 arranged on the surface of the pearlescent pigment, wherein the magnetic powder coating layer 200 is a silicon dioxide layer containing magnetic nano iron powder 210. The magnetic powder coating layer is prepared by a sol-gel method without high-temperature calcination.
The preparation method of the magnetic pearlescent pigment provided by the invention comprises the following steps:
s1, grinding and dispersing the magnetic nano iron powder raw material, tetraethyl orthosilicate and a silane coupling agent together to obtain nano iron powder with the surface grafted with the silane coupling agent, wherein the grafted nano iron powder is uniformly and stably dispersed in the tetraethyl orthosilicate;
s2, mixing the pearlescent pigment with an alcohol organic solvent, adding an alkaline catalyst, stirring and heating, adding the tetraethyl orthosilicate solution which is obtained in the step S1 and is uniformly and stably dispersed with the grafted nano iron powder, reacting together, and filtering, washing and drying to obtain the pearlescent iron powder.
Step S2 may be further refined as: mixing the traditional pearlescent pigment in an alcohol (ethanol, butanol, isopropanol and the like) organic solvent, adding an alkaline catalyst (ammonia water, ethylenediamine and the like), stirring and heating to 65-80 ℃, adding the treated nano iron tetraethyl orthosilicate mixed solution (namely the tetraethyl orthosilicate solution in which the grafted nano iron powder is uniformly and stably dispersed) obtained in the step S1 within 1-2 hours, continuously maintaining the temperature of 65-80 ℃ after the addition for stirring for 2-6 hours for reaction, filtering, washing and drying to obtain the magnetic pearlescent pigment with the surface coated with the silicon dioxide layer containing the magnetic nano iron powder.
In the above steps S1 and S2, the proportion relationship between the materials is as follows:
based on 100 parts by weight of the pearlescent pigment as raw material:
magnetic nano iron powder (primary particle size is 10-50 nm): 2-10 parts by weight; less than 2 parts by weight, the magnetic properties are weak; if the weight ratio is more than 10 parts, the coating is too much, so that the surface of the pigment is rough and the appearance effect is influenced;
tetraethyl orthosilicate: 20-100 parts by weight: when the amount is less than 20 parts by weight, the silica layer is thin and is insufficient to properly wrap the nano iron on the surface of the pigment; when it is more than 100 parts by weight, the surface of the pigment is rough and the pigment tends to aggregate; since the relative molecular weight of tetraethyl orthosilicate is 208.33 and the relative molecular weight of silica is 60, 1 part by weight of tetraethyl orthosilicate can be converted to 60/208.33 to 0.288 parts by weight of silica after the coating reaction process; 5.76 to 28.8 parts by weight of silicon dioxide is finally obtained according to 20 to 100 parts by weight of tetraethyl orthosilicate;
silane coupling agent: the chemical formula is Y-R-Si (OR)3(wherein Y is an organofunctional group, SiOR is a siloxy group); wherein the organic functional group can be amino, epoxy, acryloxy and the like, and the addition amount is 0.2 to 1 percent of the weight of the magnetic nano iron powder;
the alcohol solvent can be ethanol, n-butanol or isopropanol, and can be one or more of mixed solvents, and the mixing ratio is not required;
the alkali catalyst can be alkaline reagents such as ammonia water, triethylamine, ethylenediamine or tributylamine, etc., and is prepared into 10% aqueous solution by mass concentration, and 20-80 parts by weight of the aqueous solution is added;
the raw material of the pearlescent pigment can be common pearlescent pigments on the market, and can also be conventional pearlescent pigments produced by Zhejiang Rui New Material GmbH:
the mark KW103 is natural mica pearlescent pigment coated with titanium dioxide, and is silvery white with particle size distribution of 10-60 microns;
the mark KW205 is titanium dioxide coated natural mica pearlescent pigment with interference gold color and particle size distribution of 10-60 microns;
the mark KW225 is natural mica pearlescent pigment coated with titanium dioxide, interference blue, and the particle size distribution is 10-60 microns;
the mark KW235 is natural mica pearlescent pigment coated with titanium dioxide, interference green color, and particle size distribution of 10-60 microns;
the brand KW305 is natural mica pearlescent pigment coated with titanium dioxide and ferric oxide, which has golden color and particle size distribution of 10-60 microns;
the mark KW504 is iron sesquioxide coated natural mica pearlescent pigment with red color and particle size distribution of 10-60 microns.
In order that the objects, features and advantages of the invention will be readily apparent, a more particular description of embodiments of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings, which are included to provide a further understanding of the invention. Accordingly, the invention is not limited by the specific implementations disclosed below.
Example 1
In this embodiment, the preparation method of the magnetic pearlescent pigment includes the following steps:
s1, uniformly mixing 5g of metal iron powder with the primary particle size of 25nm, 84g of tetraethyl orthosilicate and 0.025g of silane coupling agent NQ-55 (3-aminopropyltriethoxysilane), placing the mixture in a planetary ball mill, adding 200g of zirconia balls (the diameter of 0.7 mm), grinding for 2 hours, discharging the mixture through a 100-mesh screen, and removing the zirconia balls to obtain the mixed solution of the metal iron and the tetraethyl orthosilicate with the treated surfaces. In the grinding process, partial polar groups such as hydroxyl groups on the surface of the iron powder react with ethoxy groups or aminopropyl groups, and siloxane groups are grafted on the surface of the iron powder and can be stably dispersed in tetraethyl orthosilicate so as to facilitate subsequent reaction.
S2, dispersing 100g of titanium dioxide coated natural mica pearlescent pigment KW103 (particle size distribution: 10-60 μm, Zhejiang Ruihei new materials Co., Ltd.) in 400mL of isopropanol, adding 30mL of ethylenediamine aqueous solution with the mass concentration of 10%, stirring and heating to 70 ℃, adding the mixed solution of the grafted iron powder and tetraethyl orthosilicate obtained in the step S1 within 1-2 hours, and continuously stirring for 3-6 hours at 70 ℃; cooling to room temperature, filtering the product with Buchner funnel or other filtering means (centrifugal separation, etc.), washing with small amount of isopropanol, and drying at 100-; finally obtaining the pearlescent pigment coated with the nano metallic iron on the surface.
According to theoretical calculation, in the magnetic pearlescent material obtained in the embodiment, the pearlescent pigment, the magnetic nano iron powder and the silicon dioxide are in percentage by weight: 100/(24.192+5+100): 5/(24.192+5+100): 24.192/(24.192+5+100), namely the weight percentages of the pearlescent pigment, the magnetic nanometer iron powder and the silicon dioxide are as follows: 77.4%: 3.87%: 18.73 percent.
Comparative example 1
Magnetic pearlescent pigments coated with ferroferric oxide were prepared according to the method of patent CN 102766357A. 50g of titanium dioxide-coated natural mica pearlescent pigment KW103 (particle size distribution: 10-60 μm, product of Zhejiang Rui, New materials Co., Ltd.) and a proper amount of water were poured into a 1000mL three-necked flask, water was added to 600mL scale positions, and then stirred to uniformly disperse the pearlescent pigment, and the temperature was raised to 80 ℃ and maintained. The three-necked flask was charged with nitrogen gas at a rate of 0.2L/min to displace the air in the three-necked flask. Then under nitrogen atmosphere, 20mL of a 300g/L ferrous chloride solution was added, and a sodium hydroxide solution was added to adjust the pH to 6. 23.6mL of potassium chlorate solution with the concentration of 30g/L is dripped, and part of Fe is removed by the potassium chlorate2+Is oxidized into Fe3+And cooling after the reaction is finished. The product was filtered with a buchner funnel and the filter cake rinsed with deionized water, the filter cake was re-placed into a 1000mL beaker, water was added to 700mL level and the temperature was raised to 80 ℃. 165mL of sodium silicate solution and 27.5mL of aluminum chloride solution were slowly added dropwise, stirred and the pH was maintained at 7 with 5% hydrochloric acid, after stirring for half an hour, suction filtered and the filter cake was rinsed 6 times with deionized water. The filter cake was dried at 105 ℃ and then calcined at 560 ℃ for 30 minutes under nitrogen atmosphere to obtain the final product.
Experiment:
the magnetic pearlescent pigment can be magnetically characterized by adopting the following method:
referring to fig. 2, two electronic balances are horizontally placed side by side (in parallel), a flat plate (plastic plate) is erected on the electronic balances to serve as a connecting bridge, a plastic cup is placed in the middle of the flat plate, and 5g of magnetic pearlescent pigment is contained in the plastic cup; after the two electronic balances are reset, a magnet is placed under the plastic cup (not contacting the plastic cup, refer to fig. 2), the electronic balance displays a datum due to the attraction of the magnet, the two data are added to obtain a magnetic value, and the method can be used for comparing the magnetic strength of different magnetic pearlescent pigments in parallel.
Through the test of the method, the magnetic value of the magnetic pearlescent pigment obtained by the invention is 100-120, the magnetic value of the magnetic pearlescent pigment obtained in example 1 is 100, and the magnetic value of the magnetic pearlescent pigment obtained in comparative example 1 is 43.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (9)

1. A magnetic pearlescent pigment, characterized by: the pearlescent pigment coating layer is a silicon dioxide layer with uniformly dispersed magnetic powder, the magnetic powder is magnetic nano iron powder, the silicon dioxide layer containing the magnetic powder is prepared by a sol-gel method without high-temperature calcination, and the coating process comprises the following steps:
s1, grinding and dispersing the raw material of the magnetic powder, tetraethyl orthosilicate and silane coupling agent together to obtain the magnetic powder with the surface grafted with the silane coupling agent, wherein the grafted magnetic powder is uniformly and stably dispersed in the tetraethyl orthosilicate;
s2, mixing the pearlescent pigment and the alcohol organic solvent, adding an alkaline catalyst, stirring and heating, adding the tetraethyl orthosilicate solution which is obtained in the step S1 and is uniformly and stably dispersed with the grafted magnetic powder, reacting together, filtering, washing and drying to obtain the pearlescent pigment.
2. The magnetic pearlescent pigment of claim 1, characterized in that: the pearlescent pigment is prepared by coating mica or glass or silicon dioxide or aluminum oxide flaky base materials with metal oxides.
3. The magnetic pearlescent pigment of claim 2, characterized in that: the metal oxide is titanium dioxide, or titanium dioxide and ferric oxide, or ferric oxide.
4. The magnetic pearlescent pigment of claim 3, characterized in that: the particle size of the pearlescent pigment is 5-1000 μm.
5. The magnetic pearlescent pigment of claim 1, characterized in that: in the coating process, the addition amounts of the pearlescent pigment, the magnetic powder raw material and tetraethyl orthosilicate are as follows according to parts by weight: 100 parts by weight, 2-10 parts by weight and 20-100 parts by weight.
6. The magnetic pearlescent pigment of claim 1, characterized in that: in step S1, the magnetic powder raw material is magnetic nano iron powder with a particle size of 10-50 nm.
7. The magnetic pearlescent pigment of claim 1, characterized in that: in step S2, the alcohol organic solvent is one or more of ethanol, butanol, and isopropanol.
8. The magnetic pearlescent pigment of claim 1, characterized in that: in step S2, the basic catalyst is ammonia water or aqueous solution of ethylenediamine or triethylamine or tributylamine, the temperature is raised to 65-80 ℃ by stirring, and the reaction time of the joint reaction is 2-6 hours.
9. The magnetic pearlescent pigment of claim 1, characterized in that: in step S1, the amount of the silane coupling agent added is 0.2% to 1% of the weight of the magnetic nano iron powder.
CN202110830795.9A 2021-07-22 2021-07-22 Magnetic pearlescent pigment and preparation method thereof Active CN113527914B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110830795.9A CN113527914B (en) 2021-07-22 2021-07-22 Magnetic pearlescent pigment and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110830795.9A CN113527914B (en) 2021-07-22 2021-07-22 Magnetic pearlescent pigment and preparation method thereof

Publications (2)

Publication Number Publication Date
CN113527914A CN113527914A (en) 2021-10-22
CN113527914B true CN113527914B (en) 2022-05-27

Family

ID=78120506

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110830795.9A Active CN113527914B (en) 2021-07-22 2021-07-22 Magnetic pearlescent pigment and preparation method thereof

Country Status (1)

Country Link
CN (1) CN113527914B (en)

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1225047A (en) * 1996-06-10 1999-08-04 日铁矿业株式会社 Powder coated with multilayer film and process for preparing the same
CN1226193A (en) * 1996-06-10 1999-08-18 日铁矿业株式会社 Powder coated with multilayer coating
CN101445674A (en) * 2008-12-08 2009-06-03 温州大学 Magnetic pearlescent pigment and preparation method thereof
CN102766357A (en) * 2012-08-10 2012-11-07 杭州弗沃德精细化工有限公司 Method for preparing magnetic permeability pearlescent pigment
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
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
CN205635454U (en) * 2016-05-26 2016-10-12 江苏贝丽得新材料有限公司 Magnetic pearlescent pigment
CN107434923A (en) * 2016-05-26 2017-12-05 江苏贝丽得新材料有限公司 A kind of magnetic pearlescent pigment
CN109054445A (en) * 2018-07-27 2018-12-21 浙江凯色丽科技发展有限公司 The preparation method for the magnetic pearlescent pigment of resistance to medium temperature
CN109880280A (en) * 2019-03-27 2019-06-14 金旸(厦门)新材料科技有限公司 It is a kind of to exempt from spraying ABS material and preparation method thereof with 3D pearl effect
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

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1225047A (en) * 1996-06-10 1999-08-04 日铁矿业株式会社 Powder coated with multilayer film and process for preparing the same
CN1226193A (en) * 1996-06-10 1999-08-18 日铁矿业株式会社 Powder coated with multilayer coating
CN101445674A (en) * 2008-12-08 2009-06-03 温州大学 Magnetic pearlescent pigment and preparation method thereof
CN102766357A (en) * 2012-08-10 2012-11-07 杭州弗沃德精细化工有限公司 Method for preparing magnetic permeability pearlescent pigment
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
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
CN205635454U (en) * 2016-05-26 2016-10-12 江苏贝丽得新材料有限公司 Magnetic pearlescent pigment
CN107434923A (en) * 2016-05-26 2017-12-05 江苏贝丽得新材料有限公司 A kind of magnetic pearlescent pigment
CN109054445A (en) * 2018-07-27 2018-12-21 浙江凯色丽科技发展有限公司 The preparation method for the magnetic pearlescent pigment of resistance to medium temperature
CN109880280A (en) * 2019-03-27 2019-06-14 金旸(厦门)新材料科技有限公司 It is a kind of to exempt from spraying ABS material and preparation method thereof with 3D pearl effect
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

Also Published As

Publication number Publication date
CN113527914A (en) 2021-10-22

Similar Documents

Publication Publication Date Title
CN110272641B (en) Preparation method of high-dispersity pearlescent pigment, pearlescent pigment and application of pearlescent pigment
CN104893366B (en) A kind of magnetic pearlescent pigment with 3D effect and preparation method thereof
CN101445674B (en) Magnetic pearlescent pigment and preparation method thereof
US7470318B2 (en) Synthetic mica based pearlescent pigments containing ferrites
KR970001932B1 (en) Weather-resistant pearlescent pigments and process for producing the same
CN102803400B (en) Magnetic Pigments Comprising A Flaky Substrate And A Layer Of Maghemite
JP2003513139A (en) Strongly colored interference pigment
JP2022082656A (en) Effect pigment
JPH0641456A (en) Process for producing composite pigment
KR20150048588A (en) Colored glazed pigments using natural dye and method of manufacturing the same
JP2006523734A (en) Surface modification effect pigment
CN102766357A (en) Method for preparing magnetic permeability pearlescent pigment
US5827361A (en) Carbon-containing figments
JP2004520472A (en) Flaky pigment
CN100562544C (en) A kind of golden pearly pigment and production method thereof with strong metal-like
CN113527914B (en) Magnetic pearlescent pigment and preparation method thereof
CN113105756B (en) Carbon-coated titanium pearlescent pigment and preparation method thereof
US9657185B2 (en) Brilliant black pigments
JP6853352B2 (en) Black pearl luster pigment using natural charcoal and its manufacturing method
KR20150048980A (en) Iron oxide based black glazed pigments and method of manufacturing the same
WO2006032199A1 (en) A pearl pigment used for external outside
JP2016540018A (en) Cosmetic composition
CN114716847B (en) Preparation method of pearlescent pigment with flaky alpha-alumina as matrix
JP2006291156A (en) Production method of pearlescent pigment having high brilliance and pearlescent pigment produced by the production method
JP4558283B2 (en) Gold pigment and method for producing the same

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant