CN106398321A - Preparation method of green organic/inorganic composite infrared reflection pigment - Google Patents
Preparation method of green organic/inorganic composite infrared reflection pigment Download PDFInfo
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- CN106398321A CN106398321A CN201610757217.6A CN201610757217A CN106398321A CN 106398321 A CN106398321 A CN 106398321A CN 201610757217 A CN201610757217 A CN 201610757217A CN 106398321 A CN106398321 A CN 106398321A
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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
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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
- C01P2002/80—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 preparation method of a green organic/inorganic composite infrared reflection pigment belongs to the technical field of functional pigments, and is used for preparing the infrared reflection pigment with bright color, high reflectivity and excellent weatherability. The composite infrared reflection pigment with a green coloring effect and the total solar reflectivity reaching about 60% is prepared through sol-gel technology synthesis of an inorganic pigment titanium dioxide with high infrared reflectivity in a near infrared spectroscopy reflection range and an organic pigment phthalocyanine green with high permeability in the near infrared spectroscopy range for about 34 h. The reflectivity of the composite pigment in a visible wave range of 470-570 nm is 10-15%. The inorganic pigment-containing composite infrared reflection pigment has the advantages of high infrared spectrum reflectivity, high solar spectrum reflectivity and high weatherability, provides a choice for colorful demands of the appearance of a modern building, and also realizes the building energy saving purpose.
Description
Technical field
The invention belongs to functional pigment technical field is and in particular to a kind of green organic/inorganic is combined infrared reflecting paint
Preparation method.
Background technology
Solar heat reflection paint is a kind of new special coating, has heat-insulated, cooling and energy-saving effect, in petrochemical industry storage
The aspects such as tank, grain warehouse storehouse, ship vehicle, building have a good application prospect.The solar energy of white heat-reflecting insulating coating
Heat reflection is than highest, but haves such problems as that light pollution, stain resistance are poor in urban architecture large-area applications.And color is relatively
Dullness is 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.Under the conditions of color identical it is desirable to heat-reflecting material have in near-infrared region higher anti-
Penetrate rate.The key of the colored heat reflection coatings of preparation is color infrared reflection pigment development and selection.
Pigment can be divided into inorganic pigment and organic pigment by its chemical constituent difference.At present, the face in heat reflection coatings
Material is based on inorganic pigment.Inorganic pigment has the features such as reasonable heat-resisting quantity, weatherability and stronger chemical stability,
But it exists, and chromatograph is wide, coloured light is not gorgeous, the shortcomings of tinting strength, tinting power is relatively low, and many heavy metal inorganic pigments poisonous from
And more limit the practical application of inorganic pigment.Organic pigment has that chromatograph is complete, bright in colour, strong coloring force and prepare can
The advantages of control, but color stability and weather resistance are relatively poor.Colored organic infrared reflection pigment is in heat reflection coatings
Application and research are little at present.
In order to solve the problems, such as that organic pigment physical and chemical performance, weather resistance are poor and reflectance is not high, by near infrared spectrum
In the range of have high reflectance, the inorganic pigment of preferable weather resistance and color conservation degree is good, strong coloring force organic pigment
It is combined, be expected to obtain rich color and there is the composite pigment compared with high infrared reflection rate and weather resistance.
For ensureing energy-saving cool-down effect, building energy conservation heat reflection coatings do not need only have higher initial sunlight reflection
Rate is it is often more important that can keeping its higher sunlight reflectance for a long time or reducing initial reflectance to lesser extent.Good
Ageing-resistant and contaminated resistance, can not only keep preferable energy-saving effect, and can keep the appearance characteristics of coating, for
Delay aging, the raising coating weatherability of coating, it may have important effect.
Content of the invention
The present invention provides a kind of green organic/inorganic to be combined near-infrared reflection pigment and preparation method thereof, and described green is near
With advantage of lower cost and bright organic phthalocyanine green now develops the color pigment, with high reflectance infrared reflecting paint for principal phase
It is inorganic bag nuclear material with the titanium dioxide of preferable weather resistance.This composite pigment takes into account the bright colors of organic pigment, may be used again
To have both the ageing-resistant stability characteristic (quality) of inorganic pigment moreover it is possible to properly increase reflectance.
Green organic/inorganic proposed by the invention is combined infrared reflecting paint preparation method, and know-why is as follows：
This experiment, using butyl titanate (TBOT) as presoma, carries out TiO by hydrolytic process to organic pigment particles2
Bag core.TBOT is dissolved in formation homogeneous phase solution in alcoholic solvent, TBOT occurs hydrolysis with water, dehydration occurs simultaneously 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 atomicity of metal), anti-with water
Should：Ti(OC4H9)4+x H2O→Ti(OH)x(OC4H9)4-x+x C4H9OH, reaction is persistently carried 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, comprises the following steps (see Fig. 1)：
Step 1：Solution mixes.Weigh the TBOT that volume is 13～14 parts, measure 80 parts of ethanol, 1～2 part of peracetic acid formulation becomes
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
Requirement allotment according to composite pigment colourity, reflectance), using magnetic agitation 30min so as to be dispersed in step 1 gained
Mixed solution in.
Step 3：Prepared by wet gel.Be added dropwise over acetic acid that volume is 8 parts in the sample that step 2 obtains and 10 parts go from
Sub- water, there are hydrolysis in stirring 15min.
Step 4：It is aged, be dried.The collosol intermixture that step 3 is obtained is placed on ageing 18 ± 2h shape in 50 ± 5 DEG C of water-baths
Become wet gel, after 12h being dried at 80 DEG C, obtain xerogel solid.
Step 5：Grind.The solid reactant that step 4 is obtained grinds, and obtains final organic/inorganic composite green closely red
External reflectance pigment.
The experimental evaluation that the present invention adopts includes：Colourity, visible ray/near infrared spectrum reflectance, X-ray diffraction characteristic and
FTIR spectrum；From ATLAS Ci4000 aging tester, ageing properties test is carried out 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 is 600h, and according to ageing time, timing is taken out sample and surveyed
Its colourity fixed and reflectance, characterize the ageing-resistant performance of material by the change of the colourity of comparative sample, reflectance.
The principal character of the present invention is as follows：
(1) 470nm～570nm wave band internal reflection rate in visible-range for the composite pigment is 10%～15%, color
Show as green (see Fig. 2), the color lightness of gained composite pigment, saturation and TiO2The direct phase with the mass ratio of phthalocyanine green
Close, therefore the present invention can achieve that a series of different green organic/inorganic of depths is combined the preparation of infrared reflecting paint.
(2) reflectance near infrared spectral range for the composite pigment is with TiO2Increase with the mass ratio of phthalocyanine green and carry
Height, works as TiO2Mass ratio 1 with phthalocyanine green:When 1 (embodiment 3), reflectance increase rate is about 10%, can reach 60% left
Right.
(3) titanium dioxide that the organic/inorganic of sol-gal process preparation is combined in infrared reflecting paint structure is in no
Setting state (see Fig. 3).
(4) organic pigment and inorganic TiO in composite pigment structure2Between in 1548cm-1There is Ti-H key characteristic peak in left and right,
Thus combine more closely (see Fig. 4).
(5) the ageing-resistant stability of composite pigment is preferable (see Fig. 5).
The present invention adopts sol-gal process to prepare organic/inorganic and is combined infrared reflecting paint it is intended to nanoscale
TiO2It is combined with phthalocyanine green pigment, thus forming more complete bag core and improving colourity retentivity and the combination of composite pigment
Power.Selection of the present invention easily obtains, and technological operation is easily achieved, and synthetic product Stability Analysis of Structures is it is easy to promoting and realizing industrialization.
Brief description
Fig. 1 is combined the preparation technology flow chart of near-infrared reflection pigment for the green organic/inorganic that the present invention provides.
Fig. 2 is visible ray and the 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 gained pigment of the present invention.
Specific embodiment
Embodiment 1
Weigh TBOT 13.0g, measure ethanol 80mL, acetic acid 1mL is configured to mixed solution, magnetic agitation 30min, add
The green 0.53g of organic pigment phthalocyanine, stirs 30min.It is added dropwise over acetic acid 8mL and deionized water 10mL, be spaced 15min, persistently stir
Mix to mix homogeneously, put in 45 DEG C of water-baths ageing 20h and form wet gel, 80 DEG C 12h is dried after obtain xerogel, finely ground obtain
Final products.
Embodiment 2
Weigh TBOT 13.6g, measure ethanol 80mL, acetic acid 2mL is configured to mixed solution, magnetic agitation 30min, add
The green 0.40g of organic pigment phthalocyanine, stirs 30min.It is added dropwise over acetic acid 8mL and deionized water 10mL, be spaced 15min, persistently stir
Mix to mix homogeneously, put in 50 DEG C of water-baths ageing 18h and form wet gel, 80 DEG C 12h is dried after obtain xerogel, finely ground obtain
Final products.
Embodiment 3
Weigh TBOT 14.0g, measure ethanol 80mL, acetic acid 1mL is configured to mixed solution, magnetic agitation 30min, add
The green 0.32g of organic pigment phthalocyanine, stirs 30min.It is added dropwise over acetic acid 10mL and deionized water 10mL, be spaced 15min, persistently stir
Mix to mix homogeneously, put in 50 DEG C of water-baths ageing 20h and form wet gel, 80 DEG C 12h is dried after obtain xerogel, finely ground obtain
Final products.
Gained pigment uses HP-200 type Portable precise color difference meter to measure the colourity of embodiment 1,2,3 pigment, such as table 1.
Table 1：Embodiment 1,2,3 chromatic value
| Numbering | 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, with the visible ray of UV-NIR-VIS spectrophotometer measurement pigment and near infrared spectrum reflectance, is such as schemed
Shown in 2.Tested with X-ray diffraction method (XRD), be embodiment 1,2,3 gained pigment diffracting spectrum shown in Fig. 3, gained
Collection of illustrative plates is contrasted with standard card, TiO in pigment2For amorphous state.Gained pigment structure is tested with FTIR spectrum, such as schemes
Shown in 4.
Claims (1)
1. a kind of green organic/inorganic is combined the preparation method of infrared reflecting paint it is characterised in that comprising the following steps：
Step 1：Solution mixes
Weigh the TBOT that volume is 13～14 parts, measure 80 parts of ethanol, 1～2 part of peracetic acid formulation becomes 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 of step 1 gained；
Step 3：Prepared by wet gel
It is added dropwise over acetic acid that volume is 8 parts and 10 parts of deionized waters in the sample that step 2 obtains, stirring 15min occurs water
Solution reaction obtains collosol intermixture；
Step 4：It is aged, be dried
The collosol intermixture that step 3 is obtained is placed on ageing 18 ± 2h in 50 ± 5 DEG C of water-baths to form wet gel, through dry at 80 DEG C
Xerogel solid is obtained after dry 12h；
Step 5：Grind
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 |
|---|---|---|---|
| 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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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| Publication Number | Publication Date |
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| CN106398321A true CN106398321A (en) | 2017-02-15 |
| CN106398321B CN106398321B (en) | 2018-10-19 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116445008A (en) * | 2023-03-22 | 2023-07-18 | 映泽新材料(深圳)有限公司 | Preparation method of near infrared reflective pigment |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1480492A (en) * | 2002-07-18 | 2004-03-10 | 日本化学工业株式会社 | Modified red phosphorus, its mfg. process discoloured red phosphorus compsns and fire-retardant polymeric compsn. |
| CN101870827A (en) * | 2010-05-28 | 2010-10-27 | 北京化工大学 | Preparation method of stable double-particle system electronic ink display solution |
| CN103923506A (en) * | 2014-04-12 | 2014-07-16 | 北京工业大学 | Black infrared reflection pigment and preparation method thereof |
-
2016
- 2016-08-29 CN CN201610757217.6A patent/CN106398321B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1480492A (en) * | 2002-07-18 | 2004-03-10 | 日本化学工业株式会社 | Modified red phosphorus, its mfg. process discoloured red phosphorus compsns and fire-retardant polymeric compsn. |
| CN101870827A (en) * | 2010-05-28 | 2010-10-27 | 北京化工大学 | Preparation method of stable double-particle system electronic ink display solution |
| CN103923506A (en) * | 2014-04-12 | 2014-07-16 | 北京工业大学 | Black infrared reflection pigment and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| XIAOJUAN FENG等: "Solar Reflection Characteristics of Phthalocyanine Green/TiO2 Composite Green Pigments Prepared via Different Approaches", 《MATERIALS SCIENCE FORUM》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116445008A (en) * | 2023-03-22 | 2023-07-18 | 映泽新材料(深圳)有限公司 | Preparation method of near infrared reflective pigment |
| CN116445008B (en) * | 2023-03-22 | 2024-06-07 | 映泽新材料(深圳)有限公司 | Preparation method of near infrared reflective pigment |
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| CN106398321B (en) | 2018-10-19 |
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