CN106398321B - A kind of preparation method of the compound infrared reflecting paint of green organic/inorganic - Google Patents
A kind of preparation method of the compound infrared reflecting paint of green organic/inorganic Download PDFInfo
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- CN106398321B CN106398321B CN201610757217.6A CN201610757217A CN106398321B CN 106398321 B CN106398321 B CN 106398321B CN 201610757217 A CN201610757217 A CN 201610757217A CN 106398321 B CN106398321 B CN 106398321B
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- 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
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- 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
- C09C1/3669—Treatment with low-molecular organic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/02—Amorphous compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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Abstract
A kind of preparation method of the compound infrared reflecting paint of green organic/inorganic, belongs to functional pigment technical field, prepares infrared reflecting paint that is a kind of with bright colors, while possessing high reflectance and excellent weather resistance energy.The pigment select near infrared spectrum reflected range with compared with the inorganic pigment titanium dioxide of high infrared reflection rate near infrared spectral range with green compared with the organic pigment phthalocyanine of high-permeability, sol-gel processing generated time counts roughly 34h, be prepared reach with green coloring effect, total solar reflectivity 60% or so compound infrared reflecting paint.The composite pigment is 10%~15% in visible light wave range 470nm~570nm wave band internal reflection rates.The compound infrared reflecting paint that inorganic pigment participates in has higher reflection infrared spectrum rate and solar spectrum reflectivity, is provided simultaneously with higher weather resistance.The present invention provides a kind of selection for modern architecture colorful appearance demand, and achievees the purpose that building energy conservation.
Description
Technical field
The invention belongs to functional pigment technical fields, and in particular to a kind of compound infrared reflecting paint of green organic/inorganic
Preparation method.
Background technology
Solar heat reflection paint is a kind of new special coating, has heat-insulated, cooling and energy-saving effect, is stored up in petrochemical industry
Tank, grain warehouse library, ship vehicle, building etc. have a good application prospect.The solar energy of white heat-reflecting insulating coating
Heat reflection ratio highest, but in urban architecture large-area applications there are light pollution, stain resistance is poor the problems such as.And color is opposite
It is dull, it is difficult to meet the requirement of modern architecture colorful appearance.In solar heat reflection paint, infrared reflecting paint is to determine heat
The main factor of reflecting properties.Color under the same conditions, it is desirable that heat-reflecting material has higher anti-in near-infrared region
Penetrate rate.The key for preparing colored heat reflection coatings is color infrared reflection pigment development and selection.
Pigment can be divided into inorganic pigment and organic pigment by its chemical constituent difference.Currently, the face in heat reflection coatings
Material is based on inorganic pigment.Inorganic pigment has the features such as relatively good heat-resisting quantity, weatherability and stronger chemical stability,
But its there are chromatographies it is wideless, coloured light is not gorgeous enough, and tinting strength, tinting power is relatively low the shortcomings of, and many heavy metal inorganic pigments it is toxic from
And more limit the practical application of inorganic pigment.Organic pigment has complete chromatography, bright in colour, strong coloring force and preparation can
The advantages that control, but color stability and weather resistance are relatively poor.Colored organic infrared reflects pigment in heat reflection coatings
Using and research at present it is seldom.It, will in order to solve the problems, such as that organic pigment physical and chemical performance, weather resistance are poor and reflectivity is not high
Possess high reflectance, the inorganic pigment of preferable weather resistance near infrared spectral range and color conservation degree is good, strong coloring force
Organic pigment carry out compound, be expected to obtain rich in color and with the composite pigment compared with high infrared reflection rate and weather resistance.
To ensure that energy-saving cool-down effect, building energy conservation do not need only to have higher initial sunlight reflection with heat reflection coatings
Rate, it is often more important that its higher sunlight reflectivity can be kept for a long time or reduce initial reflectance to lesser extent.It is good
Ageing-resistant and contaminated resistance can not only keep preferable energy-saving effect, and can keep the appearance characteristics of coating, for
Delay the aging of coating, improve coating weatherability, it may have important role.
Invention content
The present invention provides compound near-infrared reflection pigment of a kind of green organic/inorganic and preparation method thereof, and the green is close
Infrared reflecting paint now develops the color pigment using advantage of lower cost and bright organic phthalocyanine green as main phase, with high reflectance
Titanium dioxide with preferable weather resistance is inorganic packet nuclear material.The composite pigment takes into account the bright colors of organic pigment, and can
To have both the ageing-resistant stability characteristic (quality) of inorganic pigment, moreover it is possible to properly increase reflectivity.
The compound infrared reflecting paint preparation method of green organic/inorganic proposed by the invention, technical principle are as follows：
This experiment carries out TiO using butyl titanate (TBOT) as presoma, by hydrolytic process to organic pigment particles2
Packet core.TBOT is dissolved in alcoholic solvent and forms homogeneous phase solution, with water hydrolysis occurs for TBOT, while dehydration occurs and loses alcohol contracting
Poly- reaction, forms colloidal sol.Aged, colloidal sol forms three-dimensional network and forms gel, and desiccant gel obtains xerogel, reaction mechanism
It is divided into two steps.
Hydrolysis：Unionized formula molecule predecessor, such as metal alkoxide M (OR)n(n is the valence of metal), it is anti-with water
It answers：Ti(OC4H9)4+x H2O→Ti(OH)x(OC4H9)4-x+x C4H9OH reacts lasting and carries out to generation Ti (OH)2。
Polycondensation reaction can be divided into：Lose alcohol condensation：-Ti-OH+Ti-OC4H9-→-Ti-O-Ti-+C4H9OH；Dehydration is condensed：-
Ti-OH+Ti-OH-→-Ti-O-Ti-+H2O。
A kind of preparation method of green near-infrared reflection pigment, includes the following steps (see Fig. 1)：
Step 1：Solution mixes.It is 13~14 parts of TBOT to weigh volume, measure 80 parts of ethyl alcohol, 1~2 part of peracetic acid formulation at
Mixed solution, magnetic agitation 30min obtain homogeneous phase mixed solution to be hydrolyzed.
Step 2：Pigment disperses.With certain TiO2With the mass ratio of phthalocyanine green add organic phthalocyanine green pigment (ratio according to
According to the requirement allotment to composite pigment coloration, reflectivity), using magnetic agitation 30min, it is made to be dispersed in obtained by step 1
Mixed solution in.
Step 3：It is prepared by wet gel.Be added dropwise in the sample that step 2 obtains volume be 8 parts acetic acid and 10 parts go from
Hydrolysis occurs for sub- water, stirring 15min.
Step 4：Ageing, drying.The collosol intermixture that step 3 obtains is placed on ageing 18 ± 2h shapes in 50 ± 5 DEG C of water-baths
At wet gel, by obtaining xerogel solid after 80 DEG C of dry 12h.
Step 5：Grinding.The solid reactant grinding that step 4 is obtained, it is closely red to obtain final organic/inorganic composite green
External reflectance pigment.
The experimental evaluation that the present invention uses includes：Coloration, visible light/near infrared spectrum reflectivity, X-ray diffraction characteristic and
FTIR spectrum；ATLAS Ci4000 aging testers are selected to carry out ageing properties test to coating material, according to GB/T
1865-2009《Paint and varnish artificial weathering aging and artificial irradiation expose the xenon arc radiation of filtration to the open air》, circulation pattern setting
For 1h42min illumination, 18min illumination and spray, ageing time 600h, and according to ageing time, timing is taken out sample and is simultaneously surveyed
Its fixed coloration and reflectivity characterize the ageing-resistant performance of material by the variation of the coloration of contrast sample, reflectivity.
The main feature of the present invention is as follows：
(1) 470nm~570nm wave band internal reflection rate of the composite pigment in visible-range is 10%~15%, color
Show as green (see Fig. 2), color lightness, saturation degree and the TiO of gained composite pigment2With the direct phase of mass ratio of phthalocyanine green
It closes, therefore a series of preparation of the different compound infrared reflecting paint of green organic/inorganic of depths can be achieved in the present invention.
(2) reflectivity of the composite pigment near infrared spectral range is with TiO2Increase with the mass ratio of phthalocyanine green and carries
Height works as TiO2With the mass ratio 1 of phthalocyanine green:When 1 (embodiment 3), reflectivity increase rate is about 10%, can reach 60% left side
It is right.
(3) titanium dioxide in the compound infrared reflecting paint structure of organic/inorganic prepared by sol-gel processing is in nothing
The state that shapes (see Fig. 3).
(4) organic pigment and inorganic TiO in composite pigment structure2Between in 1548cm-1It controls there are Ti-H key characteristic peaks,
It thus combines more close (see Fig. 4).
(5) the ageing-resistant better stability of composite pigment (see Fig. 5).
The present invention prepares the compound infrared reflecting paint of organic/inorganic using sol-gel processing, it is intended to nanoscale
TiO2It is compound with phthalocyanine green pigment, to form more complete packet core and improve coloration retentivity and the combination of composite pigment
Power.Selection of the present invention easily obtains, and technological operation is easily achieved, synthetic product stable structure, easy to spread and realization industrialization.
Description of the drawings
Fig. 1 is the preparation technology flow chart of the compound near-infrared reflection pigment of green organic/inorganic provided by the invention.
Fig. 2 is the visible light and near infrared spectrum reflectance curve of embodiment 1,2,3.
Fig. 3 is the X ray diffracting spectrum of embodiment 1,2,3.
Fig. 4 is the FTIR spectrum curve of embodiment 1,2,3.
Fig. 5 is the ageing-resistant performance curve of present invention gained pigment.
Specific implementation mode
Embodiment 1
TBOT 13.0g are weighed, measure ethyl alcohol 80mL, acetic acid 1mL is configured to mixed solution, magnetic agitation 30min, addition
The green 0.53g of organic pigment phthalocyanine stirs 30min.Acetic acid 8mL and deionized water 10mL is added dropwise, is spaced 15min, persistently stirs
It mixes to being uniformly mixed, is put into 45 DEG C of water-baths and is aged 20h formation wet gels, xerogel is obtained after 80 DEG C of dry 12h, it is finely ground to obtain
Final products.
Embodiment 2
TBOT 13.6g are weighed, measure ethyl alcohol 80mL, acetic acid 2mL is configured to mixed solution, magnetic agitation 30min, addition
The green 0.40g of organic pigment phthalocyanine stirs 30min.Acetic acid 8mL and deionized water 10mL is added dropwise, is spaced 15min, persistently stirs
It mixes to being uniformly mixed, is put into 50 DEG C of water-baths and is aged 18h formation wet gels, xerogel is obtained after 80 DEG C of dry 12h, it is finely ground to obtain
Final products.
Embodiment 3
TBOT 14.0g are weighed, measure ethyl alcohol 80mL, acetic acid 1mL is configured to mixed solution, magnetic agitation 30min, addition
The green 0.32g of organic pigment phthalocyanine stirs 30min.Acetic acid 10mL and deionized water 10mL is added dropwise, is spaced 15min, persistently stirs
It mixes to being uniformly mixed, is put into 50 DEG C of water-baths and is aged 20h formation wet gels, xerogel is obtained after 80 DEG C of dry 12h, it is finely ground to obtain
Final products.
Gained pigment measures the coloration of 1,2,3 pigment of embodiment using HP-200 type Portable precise color difference meters, such as table 1.
Table 1：1,2,3 chromatic value of embodiment
| Number | L | a | b | C | H |
| Embodiment 1 | 31.43 | -5.22 | -5.39 | 7.51 | 225.91 |
| Embodiment 2 | 33.34 | -6.64 | -4.94 | 8.28 | 216.65 |
| Embodiment 3 | 33.19 | -7.27 | -6.18 | 9.54 | 220.39 |
Gained pigment is such as schemed with the visible light and near infrared spectrum reflectivity of UV-NIR-VIS spectrophotometer measurement pigment
Shown in 2.It is tested with X-ray diffraction method (XRD), is 1,2,3 gained pigment diffracting spectrum of embodiment, gained shown in Fig. 3
Collection of illustrative plates is compared with standard card, TiO in pigment2For amorphous state.Gained pigment structure is tested with FTIR spectrum, is such as schemed
Shown in 4.
Claims (1)
1. a kind of preparation method of the compound infrared reflecting paint of green organic/inorganic, it is characterised in that include the following steps：
Step 1：Solution mixes
The TBOT that volume is 13 ~ 14 parts is weighed, measures 80 parts of ethyl alcohol, 1 ~ 2 part of peracetic acid formulation into mixed solution, magnetic agitation
30min obtains homogeneous phase mixed solution to be hydrolyzed；
Step 2：Pigment disperses
By organic phthalocyanine green pigment, using magnetic agitation 30min, it is dispersed in the mixed solution obtained by step 1；
Step 3：It is prepared by wet gel
Acetic acid and the 10 parts of deionized waters that volume is 8 parts are added dropwise in the sample that step 2 obtains, water occurs for 15 min of stirring
Collosol intermixture is obtained by the reaction in solution；
Step 4：Ageing, drying
The collosol intermixture that step 3 obtains is placed in 45 ~ 50 °C of water-baths and is aged 18 ~ 20h formation wet gels, by being done at 80 °C
Xerogel solid is obtained after dry 12h；
Step 5：Grinding
The solid abrasive that step 4 is obtained obtains final organic/inorganic composite green near-infrared reflection pigment.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610757217.6A CN106398321B (en) | 2016-08-29 | 2016-08-29 | A kind of preparation method of the compound infrared reflecting paint of green organic/inorganic |
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|---|---|---|---|
| CN201610757217.6A CN106398321B (en) | 2016-08-29 | 2016-08-29 | A kind of preparation method of the compound infrared reflecting paint of green organic/inorganic |
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| CN106398321A CN106398321A (en) | 2017-02-15 |
| CN106398321B true CN106398321B (en) | 2018-10-19 |
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| JP3935012B2 (en) * | 2002-07-18 | 2007-06-20 | 日本化学工業株式会社 | Modified red phosphorus, process for producing the same, decolorized red phosphorus composition and flame retardant polymer composition |
| CN101870827B (en) * | 2010-05-28 | 2013-04-10 | 北京化工大学 | Preparation method of stable double-particle system electronic ink display solution |
| CN103923506B (en) * | 2014-04-12 | 2016-08-17 | 北京工业大学 | A kind of black infrared reflecting paint and preparation method thereof |
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