CN104830139B - Porous near-infrared reflection pigment of green and preparation method thereof - Google Patents
Porous near-infrared reflection pigment of green and preparation method thereof Download PDFInfo
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- CN104830139B CN104830139B CN201510240817.0A CN201510240817A CN104830139B CN 104830139 B CN104830139 B CN 104830139B CN 201510240817 A CN201510240817 A CN 201510240817A CN 104830139 B CN104830139 B CN 104830139B
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Abstract
The present invention discloses a kind of green porous near-infrared reflection pigment and preparation method thereof, and chemical composition is NaZn1‑x(Cr)xPO4, wherein x is 0.10~0.25.Preparation method comprises the following steps：Zinc salt and chromic salts are dissolved in deionized water in proportion, stirred at room temperature, zinc chrome solution is obtained；By the zinc chrome solution heating water bath, stirring is slowly added dropwise phosphoric acid simultaneously, obtains zinc chrome phosphorus solution；Water is dissolved in using sodium carbonate or sodium acid carbonate, sodium solution is obtained, is used as precipitating reagent；The precipitating reagent is slowly added dropwise into zinc chrome phosphorus solution, pH value is adjusted, stood, washing, alcohol is washed, dries, obtains precursor powder；The precursor powder is placed in Muffle furnace, calcined, furnace cooling, grinding obtains the green porous near-infrared reflection pigment.The pigment brightness value of the present invention is 60.27~67.34, and near-infrared sun light reflectivity is 63.84%~69.12%, is above common iron green pigment, is had broad application prospects in solar heat reflecting and heat insulating coating field.
Description
Technical field
The invention belongs to near-infrared reflection pigment technology field, and in particular to a kind of near-infrared reflection for having both loose structure
Viridine green and preparation method thereof.
Background technology
Solar heat reflecting and heat insulating coating is main to be made up of base-material, face (filling out) material and auxiliary agent etc., wherein pigment to coating every
Hot property has large effect.It can be divided into two kinds of forms of heat rejection type and heat-reflective by heat-insulated from the angle of insulating mechanism.
Heat-insulated heat rejection type is for porous material.Due to the presence in hole in porous material, the road of heat transfer is extended
Journey is so as to reduce heat transfer efficiency；The thermal conductivity factor of gas is very low in duct, and this greatly reduces heat transfer and thermal convection current again, from
And reach heat-insulated effect.
Heat-insulated heat-reflective is by having what good albedo was realized to heat radiation.In the energy of solar radiation
43% in visible light wave range, and 52% near infrared band (780-2500nm), it is seen that the heat of solar radiation concentrates on visible
Light and near infrared band.In the case that the object of same color is essentially identical to the degree of reflection of visible ray, therefore color is certain,
Improve the reflectivity of its near infrared band, it is possible to improve its albedo to heat.
However, the problem of prior art is present is：Pigment in solar heat reflecting and heat insulating coating, particularly viridine green,
Only there is certain near-infrared reflection performance, without loose structure, fail to have both that heat rejection type is heat-insulated and heat-reflective is heat-insulated
Advantage.
The content of the invention
Present invention aims at a kind of green porous near-infrared reflection pigment is prepared, gained pigment both has loose structure,
There is preferable near-infrared reflection ability again, comprehensive heat-proof quality is good.
The technical solution for realizing the object of the invention is：A kind of green porous near-infrared reflection pigment, with followingization
Learn composition：
NaZn1-x(Cr)xPO4,
Wherein x is 0.10~0.25.
Preferably, x is 0.10.
The technical solution for realizing another object of the present invention is：A kind of preparation side of green porous near-infrared reflection pigment
Method, comprises the following steps：
(31) raw material is mixed：Zinc salt and chromic salts are dissolved in deionized water in proportion, stirred at room temperature, zinc chrome is obtained molten
Liquid；
Preferably, described zinc salt includes at least one of zinc nitrate, zinc sulfate, zinc chloride, and described chromic salts includes
At least one of chromic nitrate, chromium sulfate, chromium chloride.
Preferably, the ratio of the zinc salt and chromic salts is 3~9 by the mole ratio of zinc and chromium:1.
(32) water-bath：By the zinc chrome solution heating water bath, stirring is slowly added dropwise phosphoric acid simultaneously, obtains zinc chrome phosphorus solution；
Preferably, bath temperature is 70 DEG C, and the reaction time is 1h.
(33) precipitating reagent is prepared：Water is dissolved in using sodium carbonate or sodium acid carbonate, sodium solution is obtained, is used as precipitating reagent；
Preferably, sodium carbonate or sodium bicarbonate solution concentration are 0.1~2mol/L.
(34) it is co-precipitated：The precipitating reagent is slowly added dropwise into zinc chrome phosphorus solution, pH value is adjusted, stood, washing, alcohol
Wash, dry, obtain precursor powder；
Preferably, pH value is 6~8, and drying temperature is 60~80 DEG C, and drying time is 4~10h.
(35) calcine：The precursor powder is placed in Muffle furnace, calcined, furnace cooling, grinding obtains the green
Porous near-infrared reflection pigment.
Preferably, calcining heat is 700~900 DEG C, and calcination time is 1~5h.
The present invention compared with prior art, its remarkable advantage：
(1) present invention is in visible light wave range in green, and brightness value is 60.27~67.34, bright higher than common iron green pigment
Angle value 52.05.
(2) there is loose structure：Loose structure makes it have very low thermal conductivity factor.
(3) near-infrared reflection performance is good：Near-infrared sun light reflectivity in the present invention is 63.84%~69.12%, and
The near-infrared sun light reflectivity of common iron green pigment is 62.96%, therefore the pigment of the present invention has preferable near-infrared anti-
Penetrate performance.The present invention pigment have both porous heat-insulating and heat-insulated two insulating mechanisms of near-infrared reflection, as solar heat reflection every
The composition of hot coating, can effectively improve the heat-proof quality of coating.
(4) acid-alkali-corrosive-resisting：Pigment in the present invention is to environment and human body fanout free region, with good acid-fast alkali-proof.
With reference to embodiment, the present invention is described in further detail.
Brief description of the drawings
Fig. 1 is the reacting flow chart of the preparation method of the green porous near-infrared reflection pigment of the present invention.
Fig. 2 is the green porous each embodiment raw material proportioning of near-infrared reflection pigment of the present invention, near-infrared sun light reflectivity
Table and color parameter table.
Fig. 3 is the scanning electron microscope (SEM) photograph of the green porous near-infrared reflection pigment of the present invention.
Embodiment
For ease of it is further understood that the present invention, following embodiment presses identical preparation method system
It is standby.
Raw materials are commercially available in each embodiment.
Preparation method：
First, Zn (NO are weighed in proportion3)2·6H2O and Cr (NO3)3·9H2O is dissolved in appropriate deionized water,
Stir at room temperature, solution is transferred in three-necked flask the heating water bath at 70 DEG C, measured amounts concentration is 85% phosphoric acid
It is slowly dropped in three-necked flask, stirs, reacts 1h, mixed solution is poured into beaker, 2mol/L Na is slowly added dropwise2CO3It is molten
Liquid, is stirred when being added dropwise, and regulation pH value is 7, is stood, and precipitation, suction filtration is washed with deionized 2 times, and absolute ethyl alcohol is washed 1 time,
Filter cake is placed in 70 DEG C of baking ovens and dries 6h, precursor powder is obtained, presoma is placed in 900 DEG C of calcining 2h in Muffle furnace, with
Stove is cooled down, grinding, obtains green NaZn1-x(Cr)xPO4Pigment powder.
Method of testing：To the present invention and the common iron green pigment close with color of the present invention, using the portable aberration of NH310
Instrument, selects D65 testing light sources, and 8mm measurement bores test color parameter.Using spectrophotometer test near infrared spectrum reflection
Rate, it is white calibration body to choose polytetrafluoroethylene (PTFE), and test wavelength is at intervals of 5nm.According to the spectral reflectivity of test and
GJB2502.1-2006, near-infrared sun light reflectivity is calculated using following formula.
Wherein E (λ) is corresponding energy at a length of λ of sunlight wave, and R (λ) is the spectral reflectivity that pigment is λ to wavelength.
Raw material proportioning, near-infrared sun light reflectivity and the color parameter of each embodiment are shown in accompanying drawing 2, and Fig. 3 is green for the present invention
The scanning electron microscope (SEM) photograph of the porous near-infrared reflection pigment of color.
NaZn of the present invention is can be seen that from Fig. 2 and Fig. 31-x(Cr)xPO4(x is 0.10~0.25) is green porous near-infrared
Pigment is reflected, near-infrared sun light reflectivity is 63.84%~69.12%, brightness is that 60.27~67.34, particularly x are
Effect is more preferable when 0.10.And the near-infrared sun light reflectivity of common iron green pigment is 62.96%, brightness is 52.05.
Therefore, pigment of the invention not only possesses loose structure, and has good albedo to near-infrared ripple, too
Positive heat-reflecting insulating coating field has broad application prospects.
Claims (2)
1. a kind of green porous near-infrared reflection pigment, it is characterised in that with following chemical formula：NaZn1-x(Cr)xPO4, wherein x
For 0.10.
2. a kind of preparation method of green porous near-infrared reflection pigment as claimed in claim 1, it is characterised in that including such as
Lower step：
(31) raw material is mixed：Zinc salt and chromic salts are dissolved in deionized water in proportion, stirred at room temperature, zinc chrome solution is obtained；
(32) water-bath：By the zinc chrome solution heating water bath, stirring is slowly added dropwise phosphoric acid simultaneously, obtains zinc chrome phosphorus solution；
(33) precipitating reagent is prepared：Water is dissolved in using sodium carbonate or sodium acid carbonate, sodium solution is obtained, is used as precipitating reagent；
(34) it is co-precipitated：The precipitating reagent is slowly added dropwise into zinc chrome phosphorus solution, pH value is adjusted, stood, washing, alcohol is washed, is done
It is dry, obtain precursor powder；
(35) calcine：The precursor powder is placed in Muffle furnace, calcined, furnace cooling, grinding obtains the green porous
Near-infrared reflection pigment；In (32) the water-bath step, bath temperature is 70 DEG C, and water bath time is 1h；
It is characterized in that：
In (31) the raw material blend step, described zinc salt includes at least one of zinc nitrate, zinc chloride, described chromic salts
Including at least one of chromic nitrate, chromium chloride；
In (31) the raw material blend step, it is 3~9 that the ratio of the zinc salt and chromic salts, which presses zinc and the mole ratio of chromium,:1；
Described (33) are prepared in precipitating reagent step, and sodium carbonate or sodium bicarbonate solution concentration are 0.1~2mol/L；
In (34) co-precipitation step, pH value is 6~8, and drying temperature is 60~80 DEG C, and drying time is 4~10h；
In (35) calcining step, calcining heat is 700~900 DEG C, and calcination time is 1~5h.
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| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| CN106800799A (en) * | 2016-11-28 | 2017-06-06 | 江南大学 | A kind of heat-insulated pigment of purple near-infrared high reflection |
| 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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