CN106317969A - Method for preparing coated aluminum powder pigment - Google Patents
Method for preparing coated aluminum powder pigment Download PDFInfo
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- CN106317969A CN106317969A CN201510349811.7A CN201510349811A CN106317969A CN 106317969 A CN106317969 A CN 106317969A CN 201510349811 A CN201510349811 A CN 201510349811A CN 106317969 A CN106317969 A CN 106317969A
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Abstract
The invention discloses a coated aluminum powder pigment and a preparation method thereof. The preparation method comprises the following steps: mixing the aluminum powder pigment with solvent alcohol; then adding organosiloxane, water and an acidic catalyst, carrying out heating in a water bath and carrying out a reaction so as to obtain aluminum powder pigment preliminarily coated by organosiloxane; then heating a reaction system to 65 to 120 DEG C, adding an initiator and one or a plurality of monomers containing polymerizable groups and carrying out a reaction to obtain the aluminum powder pigment coated by organosiloxane and polymer; and finally, carrying out cooling, filtering, washing and drying so as to obtain the coated aluminum powder pigment. According to the invention, organosiloxane forms a first coating layer on the surface of the aluminum powder pigment at first and then the polymer forms a second coating layer on the surface of the aluminum powder pigment, so the coated aluminum powder pigment has good acid and alkali resistance on the basis of maintenance of good metal luster and is applicable to a waterborne paint; and the method overcomes the problem of gas generation in the process of usage and storage of traditional aluminum powder pigments and lays a foundation for safe use of the aluminum powder pigment.
Description
Technical field
Invention relates to the technical field of surface of metallic pigments, specifically refers to the preparation method of a kind of coated aluminium powder pigment.
Background technology
Aluminium powder pigment is one of important metallic pigments, and main application has industrial coating, car paint, printing-ink and Plastics Processing Industry.Why aluminium powder pigment has many applications, and reason is that it has a characteristic being different from other pigment: (1) " changeable colors along with angle " effect or " double-colored " effect.When observing the coating containing aluminium powder the most from different perspectives, the color of coating can change with angle change.When coating is observed in front, coating color is the brightest；Its colour-darkening during side-looking.Aluminium powder pigment is widely used in decorative paint because of this effect.(2) aluminium powder pigment has good reflection light and the ability of reflection heat.Aluminium powder pigment can form continuous print metal film when film forming, can reflect visible ray, ultraviolet light and infrared light.Reflection to visible light full spectrum is silvery white in color, and makes it have good decoration performance；Reflection to infrared light makes it have the heat-insulating property of anti-heat；To the reflection of ultraviolet light then can protective coating will not be aging by ultraviolet damage and then extend life-span of coating.Therefore it is for petroleum industry, chemical industry and haulage vehicle, pipeline.Some hot areas abroad, aluminium powder pigment is largely used to roofing asphalt paint brush roofing, significantly reduces indoor temperature.(3) aluminium powder pigment has the covering power of variation in a big way.The technical specification expressing this performance of aluminium powder pigment is water surface covering force, and one gram of aluminium powder covering water surface can be 1000～30000cm2.Aluminium powder pigment is small aluminum scale, and its diameter and thickness have certain ratio.Thickness is less, and the little kind of diameter difference has bigger water surface covering power, and this feature does not only has its economy, and the function of glossy change.
The product major part such as coating and paint is weak acid or alkalescence, aluminium powder pigment in coating and paint is during storage or using, because being corroded by acid or alkaline matter, its color gradually can be become canescence from the metallochrome become clear, and this has had a strong impact on the performance of product.Additionally, restricted by environmental factors, coating and paint industry just develop towards the direction reducing volatile organic matter, and water paint is the reasonable selection solving this problem.When aluminium powder pigment is for water paint, many adverse influences can be produced, such as: dispersion stabilization etc..But the most important thing is, water paint is prepared the most in the basic conditions, and aluminium powder pigment is easily corroded, and its consequence not only can make aluminium powder pigment gradually lose metallic luster, and can produce substantial amounts of H2, it is susceptible to blast.Therefore, it is necessary to aluminium powder pigment is carried out surface process.
At present, the surface treatment method of aluminium powder pigment mainly has two kinds: physical protection method and chemoproection method.Physical protection method i.e. at the resin of aluminium powder surface brush layer of transparent as protective layer.Because the bonding force on resin and aluminium powder surface is more weak, therefore, resin is easy to come off from aluminium powder surface, thus loses the protective effect to aluminium powder.Chemoproection method is broadly divided into deactivation method, additive method and cladding process.Deactivation method is the method for chemical protection used the earliest, and the method is to process aluminium powder with passivator so that it is surface forms one layer of passivating film.Maximally effective passivator is chromate, but owing to environment is caused high risks by the chromium ion of sexavalence, and have carcinogenesis, therefore people are seeking new alternative method.Additive method is to add the material that aluminium powder pigment can be suppressed to corrode in the systems such as coating; to the protective effect of aluminium powder pigment, additive is that it can adsorb the surface at aluminium powder pigment; but owing to this adsorption is more weak; and additive can not completely cut off contacting of aluminium powder pigment and corrosive medium completely; thus, additive is the most very limited to the protective effect of aluminium powder pigment.Cladding process is at one or more layers more transparent material of aluminium powder pigment Surface coating, and this method is because contacting of aluminium powder pigment and corrosive medium can be completely cut off, thus can be effectively protected aluminium powder pigment from corrosion.Additionally, due to clad is transparency material, can preferably keep the distinctive gloss of aluminium powder pigment, therefore, cladding process is method the most promising in current aluminium powder surface of pigments processing method.But existing coating technology is difficult to form the protective layer of densification on aluminium powder pigment surface or protective layer is easy to come off from aluminium powder pigment surface, and aluminium powder pigment does not has preferable protective effect.
Summary of the invention
The invention aims to solve the deficiency that prior art exists, it is provided that the preparation method of a kind of coated aluminium powder pigment.Aluminium powder pigment acid and alkali-resistance, glossiness prepared by the method are good, in aqueous and solvent-based system, favorable dispersibility is preferable with Organic substance compatibilitys such as resins.
It is a further object of the present invention to provide coated aluminium powder pigment prepared by said method.
The object of the invention is achieved through the following technical solutions.
The preparation method of a kind of coated aluminium powder pigment, comprises the steps and process conditions:
The first step, in terms of mass fraction, adds 2～10 parts of aluminium powder pigments and 50～90 parts of solvent alcohols in reaction vessel, stirs 0.5～2 hour under room temperature；
Second step adds 1～10 part of organosiloxane, 4～15 parts of water, 2～8 parts of acidic catalysts in the reaction vessel described in the first step, heating in water bath, the lower reaction of stirring 2～10 hours, reaction temperature is 30～60 DEG C, regulation pH value is 4～6, obtains the aluminium powder pigment that organosiloxane is tentatively coated with；Described organosiloxane is Si (OR)4And/or R ' Si (OR)3, wherein, OR is hydrolyzable alkoxyl, and R ' is organo-functional group；
Reaction system described in second step is warming up to 65～120 DEG C by the 3rd step, add 3～20 parts of one or more monomers containing polymerizable groups, 0.01～8 part of initiator, the lower reaction of stirring 2～10 hours, obtain the aluminium powder pigment of organosiloxane and polymer overmold；The described monomer containing polymerizable groups includes styrene, divinylbenzene, acrylic acid methyl ester., methyl methacrylate, butyl methacrylate, acrylic acid, methacrylic acid, maleic anhydride or carbic anhydride；
The aluminium powder pigment suspension of the 3rd step gained is cooled to room temperature by the 4th step, then filters, and is first washed with alcohols solvent by filtering residue, then filter with after distilled water wash, then by gained filter residue and drying, baking temperature is less than 50 DEG C, drying time is 2～10 hours, obtains coated aluminium powder pigment product.
Described hydrolyzable alkoxyl is methoxy or ethoxy；Described R ' is aminopropyl, vinyl or epoxy radicals.
Described organosiloxane is tetraethoxysilane, aminopropyl triethoxysilane, vinyltrimethoxy silane or epoxy radicals trimethoxy silane.
Described styrene or divinylbenzene are the monomer containing polymerizable double bond and phenyl ring；Described acrylic acid methyl ester., methyl methacrylate or butyl methacrylate are the ester containing polymerizable double bond；Described acrylic or methacrylic acid is the acid containing polymerizable double bond；Described maleic anhydride or carbic anhydride are the anhydride containing polymerizable double bond.
Solvent alcohol used by the first step is methanol, ethanol, propanol or isopropanol.Acidic catalyst used is hydrochloric acid, phosphoric acid, sulphuric acid or Fluohydric acid..Aluminium powder pigment used is flake, and particle diameter is 100nm～50 μm.
Initiator used by 3rd step is azodiisobutyronitrile, potassium peroxydisulfate or Ammonium persulfate..
A kind of coated aluminium powder pigment prepared by said method, with aluminium powder pigment as core, organosiloxane and polymer form first, second layer of clad successively on aluminium powder pigment surface.Described aluminium powder pigment is flake, and particle diameter is 100nm～50 μm.
Aluminium powder obtained by the present invention can be made aluminium paste or use directly as aluminum pigment, there is the bin stability of excellence, in paint field such as industrial coating, metallic paint, car paints, there is preferable serviceability, when being especially applicable to water paint, there is preferable antioxidant anticorrosive performance and metallic luster keeps performance.
The present invention compared with prior art, has the advantage that and beneficial effect:
1. the present invention is in preparation process, forms one layer of clad initially with organosiloxane on aluminium powder pigment surface, and this layer of clad is stronger with the adhesion on aluminium powder pigment surface.
2. the present invention is in preparation process, on the basis of organosiloxane is tentatively coated with aluminium powder pigment, uses polymerisable monomer to be polymerized with organosiloxane, forms second layer clad, i.e. polymer covering layer.
3. the two-layer clad that organosiloxane and polymer are formed is dense, has effectively completely cut off aluminium powder pigment and other corrosive mediums, and such as the contact of oxygen gas and water, acid and alkali, the coated aluminium powder pigment that therefore prepared by the present invention has preferable acid and alkali-resistance and resistance to water.
4. the coated aluminium powder pigment that prepared by the present invention also has preferable metallic luster.
5. the Organic substances such as the resin in the coated aluminium powder pigment that prepared by the present invention and coating system have the preferable compatibility.
Detailed description of the invention
For being best understood from the present invention, below in conjunction with embodiment the present invention done and describe in detail further, but the scope of protection of present invention is not limited to the scope that embodiment represents.
Embodiment 1
The first step, in terms of mass fraction, adds 2 parts of aluminium powder pigments and 50 parts of solvent methanols in reaction vessel, stirs 0.5 hour under room temperature；
Second step adds 1 part of aminopropyl triethoxysilane, 4 parts of water, 2 parts of acidic catalyst hydrochloric acid in the reaction vessel described in the first step, heating in water bath, the lower reaction of stirring 2 hours, reaction temperature is 30 DEG C, pH value is 5, obtains the aluminium powder pigment that organosiloxane is tentatively coated with；
Reaction system described in second step is warming up to 65 DEG C by the 3rd step, adds 3 parts of styrene, 0.01 part of initiator azodiisobutyronitrile, the lower reaction of stirring 2 hours, obtains the aluminium powder pigment of organosiloxane and polymer overmold；
The aluminium powder pigment suspension of the 3rd step gained is cooled to room temperature by the 4th step, then filters.Filtering residue is first washed three times with alcohols solvent, then filters with after distilled water wash three times, then by gained filter residue and drying, baking temperature is 40 DEG C, and drying time is 2 hours, obtains final products.
Embodiment 2
The first step, in terms of mass fraction, adds 6 parts of aluminium powder pigments and 70 parts of etoh solvents in reaction vessel, stirs 1 hour under room temperature；
Second step adds 5.5 parts of tetraethoxysilanes, 9.5 parts of water, 5 parts of acidic catalyst sulphuric acid in the reaction vessel described in the first step, heating in water bath, the lower reaction of stirring 6 hours, reaction temperature is 45 DEG C, pH value is 4, obtains the aluminium powder pigment that organosiloxane is tentatively coated with；
Reaction system described in second step is warming up to 92.5 DEG C by the 3rd step, adds 5 parts of styrene and 6.5 parts of divinylbenzene, 4.005 parts of initiator potassium persulfate, the lower reaction of stirring 6 hours, obtains the aluminium powder pigment of organosiloxane and polymer overmold；
The aluminium powder pigment suspension of the 3rd step gained is cooled to room temperature by the 4th step, then filters.Filtering residue is first washed three times with alcohols solvent, then filters with after distilled water wash three times, then by gained filter residue and drying, baking temperature is 40 DEG C, and drying time is 6 hours, obtains final products.
Embodiment 3
The first step, in terms of mass fraction, adds 10 parts of aluminium powder pigments and 90 parts of solvent propanol in reaction vessel, stirs 2 hours under room temperature；
Second step adds 6 parts of epoxy radicals trimethoxy silanes, 10 parts of water, 8 parts of acidic catalyst Fluohydric acid .s in the reaction vessel described in the first step, heating in water bath, the lower reaction of stirring 10 hours, reaction temperature is 60 DEG C, pH value is 6, obtains the aluminium powder pigment that organosiloxane is tentatively coated with；
Reaction system described in second step is warming up to 120 DEG C by the 3rd step, add 5 parts of methyl methacrylates, 5 parts of first class butyl acrylate and 10 parts of acrylic acid methyl ester .s, 8 parts of initiator ammonium persulfates, the lower reaction of stirring 10 hours, obtain the aluminium powder pigment of organosiloxane and polymer overmold；
The aluminium powder pigment suspension of the 3rd step gained is cooled to room temperature by the 4th step, then filters.Filtering residue is first washed three times with alcohols solvent, then filters with after distilled water wash three times, then by gained filter residue and drying, baking temperature is 30 DEG C, and drying time is 10 hours, obtains final products.
Embodiment 4
The first step, in terms of mass fraction, adds 5 parts of aluminium powder pigments and 85 parts of solvent isopropanols in reaction vessel, stirs 1 hour under room temperature；
Second step adds 5 parts of tetraethoxysilanes, 4 parts of water, 3 parts of acidic catalyst phosphoric acid, heating in water bath in the reaction vessel described in the first step, and the lower reaction of stirring 6 hours, reaction temperature is 50 DEG C, and pH value is 5, obtains the aluminium powder pigment that organosiloxane is tentatively coated with；
Reaction system described in second step is warming up to 85 DEG C by the 3rd step, adds 4 parts of acrylic acid and 4 parts of methacrylic acids, 4 parts of initiator ammonium persulfates, the lower reaction of stirring 4 hours, obtains the aluminium powder pigment of organosiloxane and polymer overmold；
The aluminium powder pigment suspension of the 3rd step gained is cooled to room temperature by the 4th step, then filters.Filtering residue is first washed three times with alcohols solvent, then filters with after distilled water wash three times, then by gained filter residue and drying, baking temperature is 50 DEG C, and drying time is 4 hours, obtains final products.
Embodiment 5
The first step, in terms of mass fraction, adds 8 parts of aluminium powder pigments and 65 parts of solvent methanols in reaction vessel, stirs 0.5 hour under room temperature；
Second step adds 6 parts of tetraethoxysilanes, 6 parts of water, 4 parts of acidic catalyst sulphuric acid, heating in water bath in the reaction vessel described in the first step, and the lower reaction of stirring 6 hours, reaction temperature is 50 DEG C, and pH value is 4, obtains the aluminium powder pigment that organosiloxane is tentatively coated with；
Reaction system described in second step is warming up to 85 DEG C by the 3rd step, adds 10 parts of polymerisable monomer maleic anhydrides, 1 part of initiator ammonium persulfate, the lower reaction of stirring 4 hours, obtains the aluminium powder pigment of organosiloxane and polymer overmold；
The aluminium powder pigment suspension of the 3rd step gained is cooled to room temperature by the 4th step, then filters.Filtering residue is first washed three times with alcohols solvent, then filters with after distilled water wash three times, then by gained filter residue and drying, baking temperature is 50 DEG C, and drying time is 4 hours, obtains final products.
Embodiment 6
The first step, in terms of mass fraction, adds 3 parts of aluminium powder pigments and 75 parts of solvent propanol in reaction vessel, stirs 1 hour under room temperature；
Second step adds 10 parts of tetraethoxysilanes, 8 parts of water, 5 parts of acidic catalyst hydrochloric acid, heating in water bath in the reaction vessel described in the first step, and the lower reaction of stirring 6 hours, reaction temperature is 50 DEG C, and pH value is 4, obtains the aluminium powder pigment that organosiloxane is tentatively coated with；
Reaction system described in second step is warming up to 85 DEG C by the 3rd step, add 5 parts of styrene, 5 parts of methacrylic acids and 5 parts of methyl methacrylates, 4 parts of initiator ammonium persulfates, the lower reaction of stirring 4 hours, obtain the aluminium powder pigment of organosiloxane and polymer overmold；
The aluminium powder pigment suspension of the 3rd step gained is cooled to room temperature by the 4th step, then filters.Filtering residue is first washed three times with alcohols solvent, then filters with after distilled water wash three times, then by gained filter residue and drying, baking temperature is 40 DEG C, and drying time is 6 hours, obtains final products.
Claims (7)
1. a preparation method for coated aluminium powder pigment, is characterized in that comprising the steps and process conditions: the first step, in terms of mass fraction, adds 2～10 parts of aluminium powder pigments and 50～90 parts of solvent alcohols in reaction vessel, stirs 0.5～2 hour under room temperature；Second step adds 1～10 part of organosiloxane in the reaction vessel described in the first step, 4～15 parts
Water, 2～8 parts of acidic catalysts, heating in water bath, the lower reaction of stirring 2～10 hours, reaction temperature is 30～60 DEG C, and regulation pH value is 4～6, obtains the aluminium powder pigment that organosiloxane is tentatively coated with；Described organic silica
Alkane is Si (OR)4And/or R ' Si (OR)3, wherein, OR is hydrolyzable alkoxyl, and described R ' is aminopropyl, vinyl or epoxy radicals；
Reaction system described in second step is warming up to 65～120 DEG C by the 3rd step, adds 3～20 parts of one or more monomers containing polymerizable groups, 0.01～8 part of initiator, the lower reaction of stirring 2～10 hours, obtains
Organosiloxane and the aluminium powder pigment of polymer overmold；The described monomer containing polymerizable groups includes styrene, divinylbenzene, acrylic acid methyl ester., methyl methacrylate, butyl methacrylate, acrylic acid, methacrylic acid, maleic anhydride or carbic anhydride；The aluminium powder pigment suspension of the 3rd step gained is cooled to room temperature by the 4th step, then filters, by filtering residue
First wash with alcohols solvent, then filter with after distilled water wash, then by gained filter residue and drying, baking temperature is less than 50 DEG C, and drying time is 2～10 hours, obtains coated aluminium powder pigment product.
The preparation method of a kind of coated aluminium powder pigment the most according to claim 1, is characterized in that described hydrolyzable alkoxyl is methoxy or ethoxy.
The preparation method of a kind of coated aluminium powder pigment the most according to claim 1, is characterized in that described organosiloxane is tetraethoxysilane, aminopropyl triethoxysilane, vinyltrimethoxy silane or ring
Epoxide trimethoxy silane.
The preparation method of a kind of coated aluminium powder pigment the most according to claim 1, is characterized in that the solvent alcohol used by the first step is methanol, ethanol, propanol or isopropanol.
The preparation method of a kind of coated aluminium powder pigment the most according to claim 1, is characterized in that the acidic catalyst used by second step is hydrochloric acid, phosphoric acid, sulphuric acid or Fluohydric acid..
The preparation method of a kind of coated aluminium powder pigment the most according to claim 1, is characterized in that the initiator used by the 3rd step is azodiisobutyronitrile, potassium peroxydisulfate or Ammonium persulfate..
The preparation method of a kind of coated aluminium powder pigment the most according to claim 1, is characterized in that the aluminium powder pigment used by the first step is flake, and particle diameter is 100nm～50 μm.
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Cited By (10)
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| CN107099169A (en) * | 2017-05-16 | 2017-08-29 | 安徽大学 | Preparation of crosslinkable high-molecular dye and method for preparing color aluminum pigment by using crosslinkable high-molecular dye |
| CN107298876A (en) * | 2017-06-30 | 2017-10-27 | 常州创索新材料科技有限公司 | A kind of preparation method of pearlescent pigment |
| CN109306220A (en) * | 2018-09-21 | 2019-02-05 | 武汉同发科技有限公司 | A kind of water-based paint |
| CN109836853A (en) * | 2019-03-05 | 2019-06-04 | 安徽天易金属新材料有限公司 | A kind of polymer overmold aluminium pigment and preparation method thereof |
| WO2020161490A2 (en) | 2019-02-05 | 2020-08-13 | Silberline Limited | New product |
| CN111748224A (en) * | 2020-07-04 | 2020-10-09 | 上海灿达建材科技有限公司 | Aluminum powder coating for water-based paint and treatment process thereof |
| CN113150604A (en) * | 2021-03-16 | 2021-07-23 | 上海抚佳精细化工有限公司 | Printing ink and preparation method and application thereof |
| CN114292442A (en) * | 2021-12-31 | 2022-04-08 | 北京中石伟业科技股份有限公司 | Filler aluminum powder, modification method and application thereof |
| CN115197589A (en) * | 2021-04-08 | 2022-10-18 | 长沙族兴新材料股份有限公司 | Polymer-coated aluminum pigment with high metal effect and preparation method thereof |
| CN115819997A (en) * | 2022-12-13 | 2023-03-21 | 汕头市龙骅材料技术有限公司 | Preparation method of aluminum-based pearlescent pigment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107099169A (en) * | 2017-05-16 | 2017-08-29 | 安徽大学 | Preparation of crosslinkable high-molecular dye and method for preparing color aluminum pigment by using crosslinkable high-molecular dye |
| CN107099169B (en) * | 2017-05-16 | 2019-03-19 | 安徽大学 | Preparation of crosslinkable high-molecular dye and method for preparing color aluminum pigment by using crosslinkable high-molecular dye |
| CN107298876A (en) * | 2017-06-30 | 2017-10-27 | 常州创索新材料科技有限公司 | A kind of preparation method of pearlescent pigment |
| CN107298876B (en) * | 2017-06-30 | 2019-02-01 | 湖州优彩新材料股份有限公司 | A kind of preparation method of pearlescent pigment |
| CN109306220A (en) * | 2018-09-21 | 2019-02-05 | 武汉同发科技有限公司 | A kind of water-based paint |
| WO2020161490A2 (en) | 2019-02-05 | 2020-08-13 | Silberline Limited | New product |
| CN109836853A (en) * | 2019-03-05 | 2019-06-04 | 安徽天易金属新材料有限公司 | A kind of polymer overmold aluminium pigment and preparation method thereof |
| CN111748224A (en) * | 2020-07-04 | 2020-10-09 | 上海灿达建材科技有限公司 | Aluminum powder coating for water-based paint and treatment process thereof |
| CN113150604A (en) * | 2021-03-16 | 2021-07-23 | 上海抚佳精细化工有限公司 | Printing ink and preparation method and application thereof |
| CN115197589A (en) * | 2021-04-08 | 2022-10-18 | 长沙族兴新材料股份有限公司 | Polymer-coated aluminum pigment with high metal effect and preparation method thereof |
| CN115197589B (en) * | 2021-04-08 | 2023-09-22 | 长沙族兴新材料股份有限公司 | Polymer coated aluminum pigment with high metal effect and preparation method thereof |
| CN114292442A (en) * | 2021-12-31 | 2022-04-08 | 北京中石伟业科技股份有限公司 | Filler aluminum powder, modification method and application thereof |
| CN114292442B (en) * | 2021-12-31 | 2023-12-08 | 北京中石伟业科技股份有限公司 | Filler aluminum powder, modification method and application thereof |
| CN115819997A (en) * | 2022-12-13 | 2023-03-21 | 汕头市龙骅材料技术有限公司 | Preparation method of aluminum-based pearlescent pigment |
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Application publication date: 20170111 |