CN104830139A - Green porous near-infrared reflection pigment and preparation method thereof - Google Patents
Green porous near-infrared reflection pigment and preparation method thereof Download PDFInfo
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- CN104830139A CN104830139A CN201510240817.0A CN201510240817A CN104830139A CN 104830139 A CN104830139 A CN 104830139A CN 201510240817 A CN201510240817 A CN 201510240817A CN 104830139 A CN104830139 A CN 104830139A
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Abstract
The invention discloses a green porous near-infrared reflection pigment and a preparation method thereof. The chemical composition is NaZn[1-x](Cr)xPO4, wherein x is 0.10-0.25. The preparation method comprises the following steps; proportionally dissolving a zinc salt and a chromium salt in deionized water, and stirring at room temperature to obtain a zinc-chromium solution; heating the zinc-chromium solution in a water bath, and slowly and dropwisely adding phosphoric acid while stirring, thereby obtaining a zinc-chromium-phosphorus solution; dissolving sodium carbonate or sodium bicarbonate in water to obtain a sodium solution as a precipitant; slowly and dropwisely adding the precipitant into the zinc-chromium-phosphorus solution to regulate the pH value, standing, washing with water, washing with alcohol, and drying to obtain a precursor powder; and putting the precursor in a muffle furnace, calcining, carrying out furnace cooling, and grinding to obtain the green porous near-infrared reflection pigment. The brightness value of the pigment is 60.27-67.34, and the near-infrared sunlight reflectivity is 63.84-69.12%, which are respectively higher than those of the common iron green pigment. Thus, the green porous near-infrared reflection pigment has wide application prospects in the field of solar heat reflective insulation paints.
Description
Technical field
The invention belongs to near-infrared reflection pigment technology field, be specifically related to a kind of near-infrared reflection veridian having both vesicular structure and preparation method thereof.
Background technology
Solar heat reflecting and heat insulating coating is primarily of compositions such as base-material, face (filling out) material and auxiliary agents, and wherein the heat-proof quality of pigment on coating has larger impact.Heat rejection type and heat-reflective two kinds of forms can be divided into by heat insulation from the angle of insulating mechanism.
Heat rejection type is heat insulation is for porous material.Due to the existence in hole in porous material, extend heat conducting distance thus reduce heat transfer efficiency; In duct, the thermal conductivity of gas is very low, and this greatly reduces again thermal conduction and thermal convection, thus reaches heat insulation effect.
Heat-reflective is heat insulation is by there being good reflection potential to realize to thermal radiation.In the energy of solar radiation, 43% at visible light wave range, and 52% at near-infrared band (780-2500nm), and the heat of visible solar radiation concentrates on visible ray and near-infrared band.The object of same color is substantially identical to the degree of reflection of visible ray, when therefore color is certain, improves the reflectivity of its near-infrared band, just can improve its reflection potential to heat.
But prior art Problems existing is: the pigment in solar heat reflecting and heat insulating coating, particularly veridian, only there is certain near-infrared reflection performance, not there is vesicular structure, fail to have both the advantage that heat rejection type is heat insulation and heat-reflective is heat insulation.
Summary of the invention
The object of the invention is to prepare a kind of green porous near-infrared reflection pigment, and gained pigment both had vesicular structure, and have again good near-infrared reflection ability, comprehensive heat-proof quality is good.
The technical solution realizing the object of the invention is: a kind of green porous near-infrared reflection pigment, has following chemical constitution:
NaZn
1-x(Cr)
xPO
4，
Wherein x is 0.10 ~ 0.25.
Preferably, x is 0.10.
The technical solution realizing another object of the present invention is: a kind of preparation method of green porous near-infrared reflection pigment, comprises the steps:
(31) raw material mixing: zinc salt and chromic salts are dissolved in deionized water in proportion, stirred at ambient temperature, obtain zinc chrome solution;
Preferably, described zinc salt comprises at least one in zinc nitrate, zinc sulfate, zinc chloride, and described chromic salts comprises at least one in chromium nitrate, chromium sulphate, chromium chloride.
Preferably, the ratio of described zinc salt and chromic salts is 3 ~ 9:1 by the mole ratio of zinc and chromium.
(32) water-bath: by described zinc chrome solution heating in water bath, stirs and slowly drips phosphoric acid simultaneously, obtain zinc chrome phosphorus solution;
Preferably, bath temperature is 70 DEG C, and the reaction times is 1h.
(33) precipitation agent is prepared: adopt sodium carbonate or sodium bicarbonate to be dissolved in water, obtain sodium solution, as precipitation agent;
Preferably, sodium carbonate or sodium hydrogen carbonate solution concentration are 0.1 ~ 2mol/L.
(34) co-precipitation: slowly dropped to by described precipitation agent in zinc chrome phosphorus solution, adjust ph, leaves standstill, washing, and alcohol wash is dry, obtains precursor powder;
Preferably, pH value is 6 ~ 8, and drying temperature is 60 ~ 80 DEG C, and time of drying is 4 ~ 10h.
(35) calcine: described precursor powder is placed in retort furnace, calcining, furnace cooling, grinding, obtains described green porous near-infrared reflection pigment.
Preferably, calcining temperature is 700 ~ 900 DEG C, and calcination time is 1 ~ 5h.
The present invention compared with prior art, its remarkable advantage:
(1) the present invention is at visible light wave range in green, and brightness value is 60.27 ~ 67.34, higher than the brightness value 52.05 of common iron phthalocyanine.
(2) there is vesicular structure: vesicular structure makes it have very low thermal conductivity.
(3) near-infrared reflection performance is good: the near infrared sunlight reflectivity in the present invention is 63.84% ~ 69.12%, and the near infrared sunlight reflectivity of common iron phthalocyanine is 62.96%, therefore pigment of the present invention has good near-infrared reflection performance.Pigment of the present invention has both porous heat-insulating and heat insulation two insulating mechanism of near-infrared reflection, as the composition of solar heat reflecting and heat insulating coating, effectively can improve the heat-proof quality of coating.
(4) acid-alkali-corrosive-resisting: the pigment in the present invention, to environment and human body fanout free region, has good acid-fast alkali-proof.
Below in conjunction with embodiment, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the reacting flow chart of the preparation method of the present invention's green porous near-infrared reflection pigment.
Fig. 2 is each embodiment proportioning raw materials of the green porous near-infrared reflection pigment of the present invention, near infrared sunlight reflectivity table and color parameter table.
Fig. 3 is the scanning electron microscope (SEM) photograph of the present invention's green porous near-infrared reflection pigment.
Embodiment
Understand the present invention further for ease of those skilled in the art, following embodiment is all prepared by identical preparation method.
In each embodiment, raw materials is commercially available.
Preparation method:
First, Zn (NO is taken in proportion
3)
26H
2o and Cr (NO
3)
39H
2o is dissolved in appropriate deionized water, at room temperature stirs, and solution to be transferred in there-necked flask heating in water bath at 70 DEG C, measured amounts concentration be 85% phosphoric acid be slowly added drop-wise in there-necked flask, stir, reaction 1h, mixing solutions is poured in beaker, slowly drip the Na of 2mol/L
2cO
3solution, dropping limit, limit is stirred, and adjust ph is 7, leaves standstill, precipitation, suction filtration, with deionized water wash 2 times, absolute ethanol washing 1 time, is placed in 70 DEG C of dry 6h of baking oven, obtains precursor powder by filter cake, presoma is placed in retort furnace 900 DEG C calcining 2h, furnace cooling, grinding, obtains green NaZn
1-x(Cr)
xpO
4pigment powder.
Testing method: to the present invention and the common iron phthalocyanine close with color of the present invention, adopts NH310 portable colorimeter, selects D65 testing light source, 8mm calibrating, test color parameter.Adopt spectrophotometer test near infrared spectrum reflectivity, choosing tetrafluoroethylene is white calibration body, and test wavelength is spaced apart 5nm.According to spectral reflectivity and the GJB2502.1-2006 of test, utilize formulae discovery near infrared sunlight reflectivity below.
Wherein E (λ) for sunlight wavelength be energy corresponding to λ place, R (λ) for pigment be the spectral reflectivity of λ to wavelength.
The proportioning raw materials of each embodiment, near infrared sunlight reflectivity and color parameter are shown in that accompanying drawing 2, Fig. 3 is the scanning electron microscope (SEM) photograph of the present invention's green porous near-infrared reflection pigment.
As can be seen from Fig. 2 and Fig. 3, NaZn of the present invention
1-x(Cr)
xpO
4(x is 0.10 ~ 0.25) is green porous near-infrared reflection pigment, and near infrared sunlight reflectivity is 63.84% ~ 69.12%, and brightness is 60.27 ~ 67.34, better effects if when particularly x is 0.10.And the near infrared sunlight reflectivity of common iron phthalocyanine is 62.96%, brightness is 52.05.
Therefore, pigment of the present invention not only possesses vesicular structure, and has good reflection potential near infrared ripple, has broad application prospects in solar heat reflecting and heat insulating coating field.
Claims (9)
1. a green porous near-infrared reflection pigment, is characterized in that having following chemical formula: NaZn
1-x(Cr)
xpO
4, wherein x is 0.10 ~ 0.25.
2. green porous near-infrared reflection pigment as claimed in claim 1, is characterized in that: described x is 0.10.
3. a preparation method for green porous near-infrared reflection pigment as claimed in claim 1 or 2, is characterized in that, comprise the steps:
(31) raw material mixing: zinc salt and chromic salts are dissolved in deionized water in proportion, stirred at ambient temperature, obtain zinc chrome solution;
(32) water-bath: by described zinc chrome solution heating in water bath, stirs and slowly drips phosphoric acid simultaneously, obtain zinc chrome phosphorus solution;
(33) precipitation agent is prepared: adopt sodium carbonate or sodium bicarbonate to be dissolved in water, obtain sodium solution, as precipitation agent;
(34) co-precipitation: slowly dropped to by described precipitation agent in zinc chrome phosphorus solution, adjust ph, leaves standstill, washing, and alcohol wash is dry, obtains precursor powder;
(35) calcine: described precursor powder is placed in retort furnace, calcining, furnace cooling, grinding, obtains described green porous near-infrared reflection pigment.
4. the preparation method of pigment according to claim 3, it is characterized in that: in described (31) raw material mixing step, described zinc salt comprises at least one in zinc nitrate, zinc sulfate, zinc chloride, and described chromic salts comprises at least one in chromium nitrate, chromium sulphate, chromium chloride.
5. the preparation method of pigment according to claim 3, is characterized in that: in described (31) raw material mixing step, and the ratio of described zinc salt and chromic salts is 3 ~ 9:1 by the mole ratio of zinc and chromium.
6. the preparation method of pigment according to claim 3, is characterized in that: in described (32) water-bath step, bath temperature is 70 DEG C, and water bath time is 1h.
7. the preparation method of pigment according to claim 3, is characterized in that: in described (33) preparation precipitation agent step, sodium carbonate or sodium hydrogen carbonate solution concentration are 0.1 ~ 2mol/L.
8. the preparation method of pigment according to claim 3, is characterized in that: in described (34) co-precipitation step, pH value is 6 ~ 8, and drying temperature is 60 ~ 80 DEG C, and time of drying is 4 ~ 10h.
9. the preparation method of pigment according to claim 3, is characterized in that: in described (35) calcining step, calcining temperature is 700 ~ 900 DEG C, and calcination time is 1 ~ 5h.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106243944A (en) * | 2016-08-27 | 2016-12-21 | 南京理工大学 | Cerium/nitrogen-doped titanic acid aluminum base infrared composite material and preparation method thereof |
| CN106318161A (en) * | 2016-08-27 | 2017-01-11 | 南京理工大学 | Cerium-nitrogen-doped lanthanum titanate-based infrared composite material and preparation method thereof |
| CN106336789A (en) * | 2016-08-27 | 2017-01-18 | 南京理工大学 | Iron-nitrogen-doped cerium titanate-based infrared composite material and preparation method thereof |
| CN106366875A (en) * | 2016-08-27 | 2017-02-01 | 南京理工大学 | Iron-nitrogen-doped aluminaum titanate-based infrared composite material and preparation method thereof |
| CN106800799A (en) * | 2016-11-28 | 2017-06-06 | 江南大学 | A kind of heat-insulated pigment of purple near-infrared high reflection |
| CN106318162B (en) * | 2016-08-27 | 2019-06-21 | 南京理工大学 | Iron/nitrogen-doped titanic acid magnesium-based infrared composite material and preparation method thereof |
| CN112391066A (en) * | 2020-11-17 | 2021-02-23 | 浙大宁波理工学院 | Preparation of near-infrared reflection phosphate color pigment |
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| CN102659410A (en) * | 2012-05-25 | 2012-09-12 | 山东大学 | High near-infrared reflectivity nano-ceramic pigment and preparation method thereof |
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| JP2013159496A (en) * | 2012-02-02 | 2013-08-19 | Ishihara Sangyo Kaisha Ltd | Chromatic color rutile type titanium dioxide pigment, and method for producing the same |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106243944A (en) * | 2016-08-27 | 2016-12-21 | 南京理工大学 | Cerium/nitrogen-doped titanic acid aluminum base infrared composite material and preparation method thereof |
| CN106318161A (en) * | 2016-08-27 | 2017-01-11 | 南京理工大学 | Cerium-nitrogen-doped lanthanum titanate-based infrared composite material and preparation method thereof |
| CN106336789A (en) * | 2016-08-27 | 2017-01-18 | 南京理工大学 | Iron-nitrogen-doped cerium titanate-based infrared composite material and preparation method thereof |
| CN106366875A (en) * | 2016-08-27 | 2017-02-01 | 南京理工大学 | Iron-nitrogen-doped aluminaum titanate-based infrared composite material and preparation method thereof |
| CN106336789B (en) * | 2016-08-27 | 2019-02-22 | 南京理工大学 | Iron/nitrogen-doped titanic acid cerium base infrared composite material and preparation method thereof |
| CN106366875B (en) * | 2016-08-27 | 2019-02-22 | 南京理工大学 | Iron/nitrogen-doped titanic acid aluminium base infrared composite material and preparation method thereof |
| CN106318161B (en) * | 2016-08-27 | 2019-02-22 | 南京理工大学 | Cerium/nitrogen-doped titanic acid lanthanum base infrared composite material and preparation method thereof |
| CN106243944B (en) * | 2016-08-27 | 2019-05-07 | 南京理工大学 | Cerium/nitrogen-doped titanic acid aluminium base infrared composite material and preparation method thereof |
| CN106318162B (en) * | 2016-08-27 | 2019-06-21 | 南京理工大学 | Iron/nitrogen-doped titanic acid magnesium-based infrared composite material and preparation method thereof |
| CN106800799A (en) * | 2016-11-28 | 2017-06-06 | 江南大学 | A kind of heat-insulated pigment of purple near-infrared high reflection |
| CN112391066A (en) * | 2020-11-17 | 2021-02-23 | 浙大宁波理工学院 | Preparation of near-infrared reflection phosphate color pigment |
| CN112391066B (en) * | 2020-11-17 | 2021-11-19 | 浙大宁波理工学院 | Preparation of near-infrared reflection phosphate color pigment |
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| CN104830139B (en) | 2017-08-29 |
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