CN110330813A - A kind of colour TiO2Near-infrared reflection pigment and preparation method thereof - Google Patents

A kind of colour TiO2Near-infrared reflection pigment and preparation method thereof Download PDF

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CN110330813A
CN110330813A CN201910382579.5A CN201910382579A CN110330813A CN 110330813 A CN110330813 A CN 110330813A CN 201910382579 A CN201910382579 A CN 201910382579A CN 110330813 A CN110330813 A CN 110330813A
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tio
pigment
ball
colour
infrared
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CN110330813B (en
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袁乐
卿小龙
毕美
翁小龙
黄刚
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Sichuan Zhiyi Industry Co Ltd
University of Electronic Science and Technology of China
Xihua University
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Sichuan Zhiyi Industry Co Ltd
University of Electronic Science and Technology of China
Xihua University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/08—Drying; Calcining ; After treatment of titanium oxide
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT 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
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
    • C09C1/3607—Titanium dioxide
    • C09C1/3653—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT 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
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT 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
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/041—Grinding
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT 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
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/004—Reflecting paints; Signal paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/29—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for multicolour effects
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

Abstract

This application provides a kind of colour TiO2Near-infrared reflection pigment and preparation method thereof, the chemical formula of the pigment are Ti1‑m‑ nFemMonO2；The described method includes: step S1: with the TiO of preset quality score2Raw material, Fe3+Impurity and Mo6+Impurity；Step S2: the material of the outfit is successively subjected to ball milling and milled processed；Step S3: the abrasive after the milled processed is subjected to synthesis in solid state, Detitanium-ore-type is made to be fully converted to rutile-type；Step S4: by after the synthesis in solid state reactant carry out it is secondary be ground up, sieved, obtain the colour TiO2Near-infrared reflection pigment.The problems such as near infrared reflectivity that existing reflection-type energy conservation pigment can be solved by the application is low, color is single, energy-saving effect is poor.

Description

A kind of colour TiO2Near-infrared reflection pigment and preparation method thereof
Technical field
This application involves inorganic oxide near-infrared high reflection field of material technology, more particularly to a kind of colour TiO2Closely Infrared reflecting paint and preparation method thereof.
Background technique
Inorganic oxide pigments are due to being widely used in external wall, vapour with good temperature and chemical stability The fields such as vehicle, industrial equipment surface, plastics, color masterbatch, have broad application prospects.Its spectral reflection characteristic is that characterization is all kinds of One of the important parameter of inorganic pigment performance and its build-in attribute, at solar spectrum visible light wave range (400nm~700nm) Reflection characteristic directly determine the tone and lightness of pigment；Spectrum near-infrared end (700nm~2500nm) reflection characteristic with The solar heat absorption/reflection performance of pigment is closely related.At present in reaching ground total solar energy, it is seen that light area accounts for sun spoke 50% or so of firing association's energy, infrared region account for about 43%, wherein 95% infrared energy concentrate on wavelength be 0.72~ In the range of 2.5um, i.e., near infrared range.Therefore, selection has the coating of high near infrared reflectivity being capable of reflected sunlight Most of energy, reduce the temperature of body surface, avoid surface temperature increase caused by many adverse effects.
In prior art, Shen lead gift invented a kind of external wall of building high infrared reflection insulating moulding coating and preparation method thereof (in State patent CN103881484A), he, which studies, prepares reflective heat insulation pigment using titanium dioxide, and the product of invention is non-toxic, reflectivity Well.As the titanium dioxide of white pigment, although there is high reflectance (being greater than 60%) in visible light-near infrared band, Its white formed (or light color) highly-reflective coating can influence visual appearance because tone is uncoordinated with environment, and pollution resistance Difference, service life is short, is difficult to meet aesthetics of architecture requirement as energy-saving material；Currently, to the research master of near-infrared reflection pigment There are more requirements to the color of coating based on light color, however as the raising of people 's material life level.People are closeer Colored pigment is looked at, however common color pigment, to near-infrared sun light absorption more (reflectivity is low), it is color that this becomes exploitation One bottleneck of color near-infrared reflection pigment.Such as to disclose a kind of colour reflective heat-insulated by Chinese patent document CN102181217A Coating is black using ferrochrome, ferrochrome is red, five kinds of cobalt blue, titan yellow, cobalt green pigment replace the common carbon black of tradition, iron oxide red, organic The pigment such as Huang, dark green, phthalocyanine blue, although can satisfy demand of the decoration of exterior wall to color, its near-infrared that coating is made Reflectivity is relatively low (26.95%~63.16%), it is difficult to meet building energy conservation requirement.Therefore, increase the gamut of coloration of pigment and mention High near infrared band reflectivity is two important directions of current high reflection energy-saving material research.Based on the studies above direction, after Phase Sarasamma Vishnu et al. praseodymium ion prepares doping Y2Ce2O7Pigment, pigment is rendered as reddish brown after praseodymium ion doping Color, but its near infrared reflectivity only has 57.5%；Patent document CN107556801A also discloses that a kind of rust near-infrared is high Reflecting material and preparation method thereof, the rust near-infrared high reflection materials chemistry formula are Ti0.8Fe0.2O2, near-infrared reflection Rate is also only 51.28%.
In conclusion being doped to obtain color to matrix, this is the main flow direction studied at present, but mesh Pigment reflectivity made from preceding doping is relatively low, some dopant materials contain harmful heavy metal (such as cadmium red, chrome green, cobalt blue, stannic acid Cadmium, plumbous chromate etc.), it is larger to the harm of health and environment.And obtained pigment still has the single problem of color, not It is able to satisfy demand of the current coating to color.
Summary of the invention
The application provides a kind of colour TiO2Near-infrared reflection pigment and preparation method thereof, to solve existing reflection-type energy conservation The problems such as near infrared reflectivity of pigment is low, color is single, energy-saving effect is poor.
To solve the above-mentioned problems, this application discloses a kind of colour TiO2Near-infrared reflection pigment, the change of the pigment Formula is Ti1-m-nFemMonO2；Wherein, m=0.014~0.06, n=0.002~0.018.
Meanwhile disclosed herein as well is prepare above-mentioned colour TiO2The method of near-infrared reflection pigment, which comprises
Step S1: it is equipped with the TiO of preset quality score2Raw material, Fe3+Impurity and Mo6+Impurity；
Step S2: the material of the outfit is successively subjected to ball milling and milled processed；
Step S3: the abrasive after the milled processed is subjected to synthesis in solid state, Detitanium-ore-type is made to be fully converted to golden red Stone-type；
Step S4: by after the synthesis in solid state reactant carry out it is secondary be ground up, sieved, obtain the colour TiO2It is close red External reflectance pigment.
Optionally, the step S1 includes:
It is equipped with the TiO that mass fraction is 95.2%~99.1%2, 0.7%~3% Fe2O3, 0.2%~1.8% MoO3。
Preferably, the step S1 includes:
It is equipped with the TiO that mass fraction is 96.2%~99.05%2, 0.7%~3% Fe2O3, 0.25%~0.8% MoO3。
Preferably, the step S1 includes:
It is equipped with the TiO that mass fraction is 98.9%2, 0.75% Fe2O3, 0.375% MoO3。
Optionally, the step of ball-milling treatment includes:
Ball grinder is added in the material of the outfit, utilizes wet ball grinding multiple hours.
Optionally, the step of ball-milling treatment includes:
Ball grinder is added in the material of the outfit, and 50ml ethyl alcohol is added, using wet ball grinding 4 hours, material ball ratio was 1:4, revolving speed 500r/min.
Optionally, the step of milled processed includes:
By after the ball-milling treatment slurry drying, it is broken after grind.
Optionally, the step S3 includes:
Abrasive after the milled processed is put into high temperature sintering furnace, solid phase synthesis is carried out, is protected at 1000 DEG C Temperature calcining 120min, makes Detitanium-ore-type be fully converted to rutile-type.
Optionally, the step S4 includes:
Reactant after the synthesis in solid state is subjected to fine grinding, is sieved with 200 mesh filter screens, obtains the colour TiO2Near-infrared reflection pigment.
Compared with prior art, the application includes following advantages:
Propose a kind of colour TiO2The preparation method of near-infrared reflection pigment, with a variety of environment amenable element of Fe, Mo is to TiO2Pigment progress is codoping modified, passes through coloring element and adjusts Color Range and compensating elements improvement coating reflectivity Mode, improve color control range, and TiO can be kept2The high near-infrared reflection characteristic of matrix, is greatly improved pigment Solar thermal energy albedo, reduce pigment use surface heat accumulation, energy-saving coating neighborhood have wide application Prospect, and can preferably realize the harmonious of energy-saving effect and visual appearance.
Detailed description of the invention
Fig. 1 is to prepare a kind of colour TiO2The step flow chart of the method for near-infrared reflection pigment；
Fig. 2 is the colour TiO as made from different quality containing proportion2The colour table of near-infrared reflection pigment and its control group Figure；
Fig. 3 is codope TiO made from different ratio2The comparison diagram of the average reflectance of near-infrared reflection pigment；
Fig. 4~Fig. 7 is codope TiO made from different ratio2The reflectivity of near-infrared reflection pigment and its singly doping pair According to the comparison diagram of group.
Specific embodiment
In order to make the above objects, features, and advantages of the present application more apparent, with reference to the accompanying drawing and it is specific real Applying mode, the present application will be further described in detail.
Due to TiO2High refractive index crystal form (rutile-type) there are the characteristics such as good solar energy reflection effect and obtain It is widely applied, the requirement based on different application background to color and spectral reflection characteristic, if Zou J et al. is in Dyes and Pigments 109 (2014) 113-119 has delivered (Cr, Sb) the codope TiO of preparation2Pigment, using multi-component doping Method is to TiO2Pigment is modified design, and with being continuously increased for metallic element doping, paint color is from glassy yellow gradual change At orange colour, but it is gradually reduced in the reflectivity of near infrared band to 50%；Rui Yang et al. is in Solar Energy Materials&Solar Cells has been delivered Fe and N co-doped in MgTiO3In, color becomes peony from white, but Sample is only capable of reaching 53% in 700nm-2500nm wave band reflectivity.Existing codope research has some improvement, but Ideal effect is also not achieved, cannot reasonably regulate and control the relationship of color gamut and reflectivity, and higher reflection is not achieved Rate.
It is different by choosing two kinds of valence states present applicant proposes a kind of new technical solution for prior art problem Impurity (N-shaped and p-type collocation) is doped modification, serves as N-shaped (p-type) coloring impurity with a kind of nonferrous metal ion, by Impurity energy level is introduced in forbidden band and forms the characteristic absorption to low energy light photon, and then regulates and controls TiO2Color.On the other hand, In order to avoid the phenomenon that sample free carrier concentration caused by highly doped impurity concentration increases, near infrared reflectivity reduces, draw P-type (N-shaped) compensated impurity is entered, TiO is reduced by neutralizing effect2It is close red to play decrease for electronics (hole) concentration in matrix The free-carrier Absorption of wave section enhances the effect of sample near infrared reflectivity.
Embodiment:
The embodiment of the present application proposes a kind of colour TiO2Near-infrared reflection pigment, the chemical formula of the pigment are Ti1-m- nFemMonO2；Wherein, m=0.014~0.06, n=0.002~0.018.
Referring to Fig.1, while the embodiment of the present application also shows and prepares a kind of colour TiO2The method of near-infrared reflection pigment Step flow chart, the method may include:
Step S1: ingredient: it is equipped with the TiO of preset quality score2Raw material, Fe3+Impurity and Mo6+Impurity；
In one alternative embodiment of the application, it is specific to show the step S1 can include:
It is equipped with the TiO that mass fraction is 95.2%~99.1%2, 0.7%~3% Fe2O3, 0.2%~1.8% MoO3。
In one preferred embodiment of the application, the step S1 includes:
It is equipped with the TiO that mass fraction is 96.2%~99.05%2, 0.7%~3% Fe2O3, 0.25%~0.8% MoO3。
Step S2: the material of the outfit is successively subjected to ball milling and milled processed；
The step of ball-milling treatment includes:
Ball grinder is added in the material of the outfit, utilizes wet ball grinding multiple hours.
When specific implementation, it may include: ball grinder is added in the material of the outfit, and 50ml ethyl alcohol is added, using wet process Ball milling 4 hours, material ball ratio 1:4, revolving speed 500r/min.
Milled processed: by after the ball-milling treatment slurry drying, it is broken after grind.
Step S3: the abrasive after the milled processed is subjected to synthesis in solid state, Detitanium-ore-type is made to be fully converted to golden red Stone-type；
Above-mentioned steps are concretely: the abrasive after the milled processed being put into high temperature sintering furnace, solid phase conjunction is carried out At reaction, 120min is calcined in 1000 DEG C of heat preservations, Detitanium-ore-type is made to be fully converted to rutile-type.
Step S4: by after the synthesis in solid state reactant carry out it is secondary be ground up, sieved, obtain the colour TiO2It is close red External reflectance pigment.
Above-mentioned steps are concretely: the reactant after the synthesis in solid state being carried out fine grinding, with 200 mesh filter screen mistakes Sieve, obtains the colour TiO2Near-infrared reflection pigment.
According to the purpose of the application and used technological means, step S1~S4 selects Fe3+And Mo6+Codope TiO2Come Develop the colored TiO of high near infrared reflectivity2Pigment.
When the coloring impurity is Fe3+When, the compensated impurity is Mo6+；
When the coloring impurity is Mo6+When, the compensated impurity is Fe3+。
When realizing, pass through coloring impurity Fe3+(Mo6+) doping introduce impurity energy level, cause TiO2Bandwidth changes Become, causes visible absorption spectrum to change, change the color of matrix.However as the increase of coloring impurity doping concentration, The free carrier concentration that will lead in sample is increased, to reduce the near infrared reflectivity of sample.Therefore, the application introduces The high-valence state Mo of certain proportion6+(lower valency Fe3+) it is used as compensated impurity, the addition of compensated impurity can reduce the sky in matrix Cave (electronics) concentration is played the role of reducing free carrier, the near infrared reflectivity of sample is promoted with this.
Meanwhile the coloring impurity and compensated impurity of the embodiment of the present application can play regulation white TiO2Pigment it is visible The effect of optical absorption spectra and color has further widened the modification scope of color.Its unique advantage is both to improve face Color modification scope, and TiO can be kept2The solar thermal energy reflection of pigment is greatly improved in the high near-infrared reflection characteristic of matrix Ability reduces the heat accumulation that pigment uses surface, has broad application prospects in energy-saving coating neighborhood, and can be preferably Realize the harmonious of energy-saving effect and visual appearance.
Next, devising two experimental groups in order to further verify the exploitativeness of the embodiment of the present application and three right It is illustrated according to technical solution of the group to the embodiment of the present application.
Experimental group one: prepare 98.875% TiO according to mass fraction2, 0.75% Fe2O3, 0.375% MoO3；It will Ball grinder is added in the raw material of the outfit, and 50ml ethyl alcohol is added, using wet ball grinding 4 hours, material ball ratio 1:4, revolving speed 500r/min.By after ball milling slurry drying, it is broken after grind.Abrasive after grinding is put into high temperature sintering furnace, into Row solid phase synthesis calcines 120min in 1000 DEG C of heat preservations, converts rutile-type for Detitanium-ore-type.After the completion of solid phase reaction It is ground up, sieved for the second time.The reactant of synthesis in solid state is subjected to fine grinding, is sieved with 200 mesh filter screens, obtains Fe3+、 Mo6+Codope TiO2Near-infrared reflection pigment.
Experimental group two: prepare 96.75% TiO according to mass fraction2, 2.5% Fe2O3, 0.75% MoO3.By institute It states and obtains Fe not described here any more referring to experimental group one the step of the raw material of outfit is handled3+、Mo6+Codope TiO2It is close red External reflectance pigment.
Control group one: prepare 98.5%~100% TiO according to mass fraction2, prepare 0% MoO respectively3, 0.375% MoO3, 0.75% MoO3, 1.5% MoO3.Above-mentioned prepared raw material is successively labeled as sample 1-1, sample 1-2, sample Product 1-3, sample 1-4 are separately added into different ball grinders, and subsequent processing steps obtain not described here any more referring to experimental group one Mo6+Single doping TiO2Near-infrared reflection pigment.
Control group two: prepare 97.75%~99.25% TiO according to mass fraction2, 0.75% Fe2O3, prepare respectively 0% MoO3, 0.375% MoO3, 0.75% MoO3, 1.5% MoO3.Above-mentioned prepared raw material is successively labeled as Sample 2-1, sample 2-2 (i.e. experimental group one), sample 2-3, sample 2-4 are separately added into different ball grinders, subsequent processing steps Fe is obtained not described here any more referring to experimental group one3+、Mo6+Codope TiO2Near-infrared reflection pigment.
Control group three: prepare 96%~97.5% TiO according to mass fraction2, 2.5% Fe2O3, prepare 0% respectively MoO3, 0.375% MoO3, 0.75% MoO3, 1.5% MoO3.Above-mentioned prepared raw material is successively labeled as sample 3- 1, sample 3-2, sample 3-3 (i.e. experimental group two), sample 3-4 are separately added into different ball grinders, and subsequent processing steps are referring to real Group one is tested, not described here any more, obtains Fe3+、Mo6+Codope TiO2Near-infrared reflection pigment.
To sum up, the characteristics of two experimental groups and three control groups are compared, obtain the application by the embodiment of the present application packet It includes:
(1) phase structure of the pigment obtained by is rutile-type with a high refractive index, can reach good solar energy Reflecting effect.
(2) pass through Fe3+、Mo6+TiO2 near-infrared reflection pigment made from codope has plurality of color under different ratio Coloured silk, such as: red, orange, yellow, green, indigo color.Referring to fig. 2, the embodiment of the present application is shown to match by different quality containing Than colour TiO obtained2The colour table figure of near-infrared reflection pigment；The colour table figure has been subjected to gray proces in Fig. 2.
(3) single doping TiO2The average reflectance of near-infrared reflection pigment is reduced with the increase of its concentration, and the application Codope TiO2The average reflectance of near-infrared reflection pigment first rises with the increase of its concentration to be subtracted afterwards.Therefore, it need to only control altogether Doping ratio, available higher average reflectance.As one preferred embodiment of the application, being equipped with mass fraction is 98.875% TiO2, 0.75% Fe2O3, 0.375% MoO3；Under mass fraction proportion, obtained colored TiO2 Near-infrared reflection pigment, i.e. Fe3+、Mo6+Codope TiO2The average reflectance of near-infrared reflection pigment is up to 95% or more.
Referring to Fig. 3, codope TiO made from different ratio is shown2Pair of the average reflectance of near-infrared reflection pigment Than figure.In Fig. 3, what X=0 was represented is control group one；What X=0.0075 was represented is control group two；What X=0.025 was represented is pair Fe is referred to according to three, X of group2O3Mass fraction, Y indicate MoO3Mass fraction.
(4) referring to fig. 4~Fig. 7 shows codope TiO made from different ratio2The reflectivity of near-infrared reflection pigment The comparison diagram of control group is singly adulterated with it.It is learnt according to comparing result, TiO made from codope2Near-infrared reflection pigment it is anti- Rate is penetrated, it is better than the reflectivity singly adulterated in certain proportion.The X of Fig. 4~Fig. 7 refers to Fe2O3Mass fraction, Y indicate MoO3Mass fraction.
All the embodiments in this specification are described in a progressive manner, the highlights of each of the examples are with The difference of other embodiments, the same or similar parts between the embodiments can be referred to each other.
Above to a kind of colour TiO provided herein2Near-infrared reflection pigment and preparation method thereof has carried out in detail It introduces, specific examples are used herein to illustrate the principle and implementation manner of the present application, the explanation of above embodiments It is merely used to help understand the present processes and its core concept；At the same time, for those skilled in the art, according to this The thought of application, there will be changes in the specific implementation manner and application range, in conclusion the content of the present specification is not answered It is interpreted as the limitation to the application.

Claims (10)

1. a kind of colour TiO2Near-infrared reflection pigment, which is characterized in that the chemical formula of the pigment is Ti1-m-nFemMonO2；Its In, m=0.014~0.06, n=0.002~0.018.
2. preparing a kind of colour TiO described in claim 12The method of near-infrared reflection pigment, which is characterized in that the method Include:
Step S1: it is equipped with the TiO of preset quality score2Raw material, Fe3+Impurity and Mo6+Impurity；
Step S2: the material of the outfit is successively subjected to ball milling and milled processed；
Step S3: the abrasive after the milled processed is subjected to synthesis in solid state, Detitanium-ore-type is made to be fully converted to rutile-type；
Step S4: by after the synthesis in solid state reactant carry out it is secondary be ground up, sieved, obtain the colour TiO2Near-infrared is anti- Penetrate pigment.
3. according to the method described in claim 2, it is characterized in that, the step S1 includes:
It is equipped with the TiO that mass fraction is 95.2%~99.1%2, 0.7%~3% Fe2O3, 0.2%~1.8% MoO3。
4. according to the method described in claim 3, it is characterized in that, the step S1 includes:
It is equipped with the TiO that mass fraction is 96.2%~99.05%2, 0.7%~3% Fe2O3, 0.25%~0.8% MoO3。
5. according to the method described in claim 4, it is characterized in that, the step S1 includes:
It is equipped with the TiO that mass fraction is 98.9%2, 0.75% Fe2O3, 0.375% MoO3。
6. according to the method described in claim 2, it is characterized in that, the step of ball-milling treatment include:
Ball grinder is added in the material of the outfit, utilizes wet ball grinding multiple hours.
7. according to the method described in claim 6, it is characterized in that, the step of ball-milling treatment include:
Ball grinder is added in the material of the outfit, and 50ml ethyl alcohol is added, using wet ball grinding 4 hours, material ball ratio 1:4, Revolving speed is 500r/min.
8. according to the method described in claim 2, it is characterized in that, the step of milled processed include:
By after the ball-milling treatment slurry drying, it is broken after grind.
9. according to the method described in claim 2, it is characterized in that, the step S3 includes:
Abrasive after the milled processed is put into high temperature sintering furnace, solid phase synthesis is carried out, is forged in 1000 DEG C of heat preservations 120min is burnt, Detitanium-ore-type is made to be fully converted to rutile-type.
10. the method according to claim 2 or 9, which is characterized in that the step S4 includes:
Reactant after the synthesis in solid state is subjected to fine grinding, is sieved with 200 mesh filter screens, obtains the colour TiO2Closely Infrared reflecting paint.
CN201910382579.5A 2019-05-09 2019-05-09 Color TiO2Near-infrared reflection pigment and preparation method thereof Expired - Fee Related CN110330813B (en)

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