CN110028811A - A kind of high near infrared reflectivity blue pigment and preparation method thereof - Google Patents

A kind of high near infrared reflectivity blue pigment and preparation method thereof Download PDF

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CN110028811A
CN110028811A CN201910340984.0A CN201910340984A CN110028811A CN 110028811 A CN110028811 A CN 110028811A CN 201910340984 A CN201910340984 A CN 201910340984A CN 110028811 A CN110028811 A CN 110028811A
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near infrared
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high near
blue pigment
infrared reflectivity
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CN110028811B (en
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周军
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Shandong Sinocera Kang Litai New Mstar Technology Ltd
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Shandong Sinocera Kang Litai New Mstar Technology Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36Compounds of titanium
    • C09C1/3607Titanium dioxide
    • C09C1/3615Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C1/363Drying, calcination
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36Compounds of titanium
    • C09C1/3607Titanium dioxide
    • C09C1/3653Treatment with inorganic compounds
    • C09C1/3661Coating
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36Compounds of titanium
    • C09C1/3692Combinations of treatments provided for in groups C09C1/3615 - C09C1/3684
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/043Drying, calcination
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds
    • C09C3/063Coating

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  • Inorganic Compounds Of Heavy Metals (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

The present invention relates to inorganic functional pigment technology fields, and in particular to a kind of high near infrared reflectivity blue pigment and preparation method thereof, comprising the following steps: Step 1: the first suspension of preparation;Step 2: the second suspension of preparation;Step 3: combustion reaction;Step 4: calcining.The preparation method is using the rutile titanium dioxide of high near infrared reflectivity as kernel, rutile titanium dioxide surface is attached to using combustion synthesis zaffre and forms outer core, and keep the pigment granules generated tiny using combustion reaction, and it is attached to the surface of rutile titanium dioxide, form high near infrared reflectivity blue pigment.This preparation method has combustion reaction temperature low, energy conservation and environmental protection, the advantages of strong operability, by adjusting titanium ion and cobalt ions molar ratio, it can be achieved to regulate and control the shade of colorant, obtained high near infrared reflectivity blue pigment has particle tiny and is evenly distributed, the strong advantage of color development ability.

Description

A kind of high near infrared reflectivity blue pigment and preparation method thereof
Technical field
The present invention relates to inorganic functional pigment technology fields, and in particular to a kind of high near infrared reflectivity blue pigment and its Preparation method.
Background technique
Solar radiation is made of 5% ultraviolet radiation, 43% visible optical radiation and 52% near infrared radiation.It is common to build The solar radiation of 10-20% can only be reflected by building object roof, cause indoor high-temperature refrigeration costly.If reflecting 60% sun spoke It penetrates, it will save 20% or more high-temperature refrigeration energy.Therefore, it studies high near infrared reflectivity material and one is possessed for energy-saving ring Fixed meaning.
Currently, the highest material of near infrared reflectivity is titanium dioxide, but that there are colors is single, easy for titanic oxide material It is dirty, cause the problems such as light pollution;Therefore, many mechanisms start to prepare high near-infrared using solid phase calcination method or coprecipitation anti- The colorful pigment of rate is penetrated, but solid phase calcination method is there are firing temperature height, energy consumption is high, particle diameter distribution is uneven, chemical reaction is not thorough The problems such as bottom, coprecipitation is there are a large amount of waste liquids, the problem of polluting environment.
In the prior art, the relevant technologies for not finding blue near-infrared reflection pigment temporarily at present, have pertained only to salt chemical combination Object and oxide pass through coprecipitation or the other relevant pigment of Solid phase synthesis near-infrared reflection.Number of patent application is In 201510240842.9 Chinese patent " a kind of the porous near-infrared high reflection pigment of aubergine and preparation method thereof ", it is utilized Zinc salt, manganese salt, phosphoric acid and sodium carbonate or sodium bicarbonate are uniformly mixed, and prepare near-infrared reflection pigment using coprecipitation. The Chinese patent application " preparation method of the ultra-fine heat-insulated black pigment of near-infrared reflection " of number of patent application 201711370212.9 In, it is uniform using chromic salts, molysite, Doped ions salt, surfactant, precipitant mix, near-infrared is prepared using coprecipitation Reflect pigment.Chinese patent " a kind of bronzing near-infrared reflection pigment and its preparation of number of patent application 201410149298.2 Method " it is being uniformly mixed using di-iron trioxide, titanium dioxide, chrome green, aluminum oxide, using solid phase calcination method Prepare near-infrared reflection pigment.Therefore, existing near-infrared reflection pigment, it is most of to be prepared using solid phase method, there is firing temperature The defects of degree is high, distribution of particles is uneven, and coprecipitation generates a large amount of waste liquid in the fabrication process, pollutes asking for environment Topic.
Summary of the invention
It is an object of the present invention in view of the deficiencies of the prior art, provide a kind of high near infrared reflectivity blue pigment Preparation method, the preparation method have combustion reaction temperature it is low, the time is short, the advantage of production process environmental protection.
The second object of the present invention is in view of the deficiencies of the prior art, to provide a kind of high near infrared reflectivity blue face Material, the high near infrared reflectivity blue pigment have particle tiny and are evenly distributed, the strong advantage of color development ability.
One of to achieve the goals above, the present invention adopts the following technical scheme:
A kind of preparation method of high near infrared reflectivity blue pigment is provided, it the following steps are included:
Step 1: the first suspension of preparation: it is soluble in water with certain mass percent by polyvinylpyrrolidone, and With magnetic stirrer certain time, the first solution is obtained, then by rutile titanium dioxide powder with certain quality Percentage is added in the first solution, and after a certain period of time with magnetic stirrer, and it is certain to move on to ultrasonic disperser ultrasound Time forms the first suspension of stable uniform;
Step 2: the second suspension of preparation: weighing cabaltous nitrate hexahydrate according to stoichiometric ratio and ANN aluminium nitrate nonahydrate is made For oxidant, dissolved organic matter is weighed as reducing agent, then has cabaltous nitrate hexahydrate, ANN aluminium nitrate nonahydrate and solubility Machine object is dissolved in the first suspension that step 1 obtains, and is stirred, and the second suspension of stable uniform is made;
Step 3: combustion reaction: the second suspension made from step 2 is placed in electric furnace the spontaneous combustion under certain temperature It burns, held for some time after burning, after natural cooling, obtains the presoma of reaction product;
Step 4: calcining: the presoma that step 3 is obtained is calcined under certain temperature after grinding uniformly, and keeps the temperature one It fixes time, then cooled to room temperature, obtains the high near infrared reflectivity blue pigment.
It is 1%~6% molten with mass percent by polyvinylpyrrolidone in the step 1 in above-mentioned technical proposal In deionized water, and with magnetic stirrer 15min~30min, the first solution is obtained.
In above-mentioned technical proposal, in the step 1, then it is with mass percent by rutile titanium dioxide powder 2%~45% is added in the first solution, and super with ultrasonic disperser after magnetic stirrer 15min~40min, is moved on to Sound 15min~45min forms the first suspension of stable uniform.
In above-mentioned technical proposal, in the step 2, the dissolved organic matter is glycine, Beta-alanine, urea, sugarcane One of sugar or citric acid.
In above-mentioned technical proposal, in the step 2, in second suspension, the molar ratio of titanium ion and cobalt ions is 0.2~5 ︰ 1.
In above-mentioned technical proposal, in the step 2, the time of the stirring is 30min~60min.
In above-mentioned technical proposal, in the step 3, the second suspension made from step 2 is placed in electric furnace in 300 DEG C Spontaneous combustion at~500 DEG C keeps the temperature 10min~60min after burning, after natural cooling, obtain the presoma of reaction product.
In above-mentioned technical proposal, in the step 4, the presoma that step 3 is obtained, grinding uniformly after, in 900 DEG C~ It is calcined at 1100 DEG C, and keeps the temperature 60min~210min, then cooled to room temperature, obtain the high near infrared reflectivity Blue pigment.
Compared with prior art, beneficial effect is the present invention:
(1) preparation method of a kind of high near infrared reflectivity blue pigment provided by the invention, is with high near-infrared reflection The rutile titanium dioxide of rate is kernel, is attached to rutile titanium dioxide surface shape using combustion synthesis zaffre At outer core, and the amount of heat and gas released using combustion reaction, mention the own temperature moment of substance in combustion 1000 DEG C or more are risen to, the firing temperature of cobalt aluminate colorant is reached, the pigment granules for generation of burning are tiny, and be attached to The surface of rutile titanium dioxide forms high near infrared reflectivity blue pigment.In addition, this preparation method has combustion reaction Temperature is low, and the time is short, and the low advantage of calcination temperature is beneficial to energy conservation emission reduction, and technical process is simple, and strong operability is whole A process is easily controllable and realizes, production process environmental protection is conducive to large-scale promotion and application.
(2) preparation method of a kind of high near infrared reflectivity blue pigment provided by the invention, by adjusting titanium ion with Cobalt ions molar ratio can be prepared and be of different shades (by light blue to depth, it can be achieved that the shade to colorant regulates and controls It is blue) high near infrared reflectivity blue pigment.
(3) a kind of high near infrared reflectivity blue pigment provided by the invention has particle tiny and is evenly distributed, color development The strong advantage of ability.
Specific embodiment
In order to which the technical problems, technical solutions and beneficial effects solved by the present invention is more clearly understood, below in conjunction with Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only to explain this Invention, is not intended to limit the present invention.
A kind of preparation method of high near infrared reflectivity blue pigment, it the following steps are included:
Step 1: the first suspension of preparation: by polyvinylpyrrolidone, with mass percent be 1%~6% be dissolved in from In sub- water, and with magnetic stirrer 15min~30min, the first solution is obtained, then by rutile titanium dioxide powder It is added in the first solution with mass percent for 5%~45%, and with after magnetic stirrer 15min~40min, moved on to Ultrasonic disperser ultrasound 15min~45min forms the first suspension of stable uniform;
Step 2: the second suspension of preparation: weighing cabaltous nitrate hexahydrate according to stoichiometric ratio and ANN aluminium nitrate nonahydrate is made For oxidant, dissolved organic matter is weighed as reducing agent, then has cabaltous nitrate hexahydrate, ANN aluminium nitrate nonahydrate and solubility Machine object is dissolved in the first suspension that step 1 obtains, stirring 30min~60min mixing, and second that stable uniform is made is outstanding Supernatant liquid;In the present embodiment, the molar ratio of titanium ion and cobalt ions is 0.2~5 ︰ 1;
In the present embodiment, dissolved organic matter is one of glycine, Beta-alanine, urea, sucrose or citric acid;
Step 3: combustion reaction: the second suspension made from step 2 is placed in electric furnace at 300 DEG C~500 DEG C certainly Hair burns, heat preservation 10min~60min after burning, after natural cooling, obtains the presoma of reaction product;
Step 4: calcining: the presoma that step 3 is obtained is calcined at 900 DEG C~1100 DEG C after grinding uniformly, and 60min~210min is kept the temperature, then cooled to room temperature, obtains the high near infrared reflectivity blue pigment.
Embodiment 1.
A kind of preparation method of high near infrared reflectivity blue pigment, it the following steps are included:
Step 1: the first suspension of preparation: by polyvinylpyrrolidone, being dissolved in deionized water with mass percent for 1% In, and with magnetic stirrer 15min, the first solution is obtained, then by rutile titanium dioxide powder with quality percentage Number is added in the first solution for 2%, and with after magnetic stirrer 15min, moves on to ultrasonic disperser ultrasound 20min, Form the first suspension of stable uniform;
Step 2: the second suspension of preparation: weighing cabaltous nitrate hexahydrate and nine hydrations according to the introducing of stoichiometric ratio 100% Aluminum nitrate weighs dissolved organic matter as reducing agent as oxidant, then by cabaltous nitrate hexahydrate, ANN aluminium nitrate nonahydrate and Dissolved organic matter is dissolved in the first suspension that step 1 obtains, stirring 35min mixing, and second that stable uniform is made is outstanding Supernatant liquid;In the present embodiment, the molar ratio of titanium ion and cobalt ions is 0.2 ︰ 1;
In the present embodiment, dissolved organic matter is glycine, and chemical equation is as follows:
9Co(NO3)2·6H2O+18Al(NO3)3·9H2O+40C2H5NO2→9CoAl2O4+80CO2↑+316H2O+56N2
Step 3: combustion reaction: the second suspension made from step 2 is placed in electric furnace the spontaneous combustion at 380 DEG C, It keeps the temperature 25min after burning, after natural cooling, obtains the presoma of reaction product;
Step 4: calcining: the presoma that step 3 is obtained is calcined at 900 DEG C in crucible after grinding uniformly, And 90min is kept the temperature, then cooled to room temperature, obtains the high near infrared reflectivity blue pigment.
Embodiment 2.
A kind of preparation method of high near infrared reflectivity blue pigment, it the following steps are included:
Step 1: the first suspension of preparation: by polyvinylpyrrolidone, being dissolved in deionization with mass percent for 1.5% In water, and with magnetic stirrer 15min, the first solution is obtained, then by rutile titanium dioxide powder with quality hundred Score is added in the first solution for 3.5%, and ultrasonic with ultrasonic disperser after magnetic stirrer 20min, is moved on to 23min forms the first suspension of stable uniform;
Step 2: the second suspension of preparation: weighing cabaltous nitrate hexahydrate according to stoichiometric ratio and ANN aluminium nitrate nonahydrate is made For oxidant, dissolved organic matter is weighed as reducing agent, then has cabaltous nitrate hexahydrate, ANN aluminium nitrate nonahydrate and solubility Machine object is dissolved in the first suspension that step 1 obtains, and the second suspension of stable uniform is made in stirring 40min mixing;This In embodiment, the molar ratio of titanium ion and cobalt ions is 0.5 ︰ 1;
In the present embodiment, dissolved organic matter is Beta-alanine;
Step 3: combustion reaction: the second suspension made from step 2 is placed in electric furnace the spontaneous combustion at 400 DEG C, It keeps the temperature 25min after burning, after natural cooling, obtains the presoma of reaction product;
Step 4: calcining: the presoma that step 3 is obtained is calcined at 950 DEG C in crucible after grinding uniformly, And 120min is kept the temperature, then cooled to room temperature, obtains the high near infrared reflectivity blue pigment.
Embodiment 3.
A kind of preparation method of high near infrared reflectivity blue pigment, it the following steps are included:
Step 1: the first suspension of preparation: by polyvinylpyrrolidone, being dissolved in deionization with mass percent for 3.5% In water, and with magnetic stirrer 25min, the first solution is obtained, then by rutile titanium dioxide powder with quality hundred Score is added in the first solution for 10.5%, and ultrasonic with ultrasonic disperser after magnetic stirrer 30min, is moved on to 27min forms the first suspension of stable uniform;
Step 2: the second suspension of preparation: weighing cabaltous nitrate hexahydrate according to stoichiometric ratio and ANN aluminium nitrate nonahydrate is made For oxidant, dissolved organic matter is weighed as reducing agent, then has cabaltous nitrate hexahydrate, ANN aluminium nitrate nonahydrate and solubility Machine object is dissolved in the first suspension that step 1 obtains, and the second suspension of stable uniform is made in stirring 45min mixing;This In embodiment, the molar ratio of titanium ion and cobalt ions is 1.5 ︰ 1;
In the present embodiment, dissolved organic matter is urea;
Step 3: combustion reaction: the second suspension made from step 2 is placed in electric furnace the spontaneous combustion at 420 DEG C, It keeps the temperature 30min after burning, after natural cooling, obtains the presoma of reaction product;
Step 4: calcining: the presoma that step 3 is obtained is calcined at 950 DEG C in crucible after grinding uniformly, And 150min is kept the temperature, then cooled to room temperature, obtains the high near infrared reflectivity blue pigment.
Embodiment 4.
A kind of preparation method of high near infrared reflectivity blue pigment, it the following steps are included:
Step 1: the first suspension of preparation: by polyvinylpyrrolidone, being dissolved in deionized water with mass percent for 5% In, and with magnetic stirrer 30min, the first solution is obtained, then by rutile titanium dioxide powder with quality percentage Number is added in the first solution for 21%, and with after magnetic stirrer 35min, moves on to ultrasonic disperser ultrasound 32min, Form the first suspension of stable uniform;
Step 2: the second suspension of preparation: weighing cabaltous nitrate hexahydrate according to stoichiometric ratio and ANN aluminium nitrate nonahydrate is made For oxidant, dissolved organic matter is weighed as reducing agent, then has cabaltous nitrate hexahydrate, ANN aluminium nitrate nonahydrate and solubility Machine object is dissolved in the first suspension that step 1 obtains, and the second suspension of stable uniform is made in stirring 50min mixing;This In embodiment, the molar ratio of titanium ion and cobalt ions is 3 ︰ 1;
In the present embodiment, dissolved organic matter is sucrose;
Step 3: combustion reaction: the second suspension made from step 2 is placed in electric furnace the spontaneous combustion at 450 DEG C, It keeps the temperature 40min after burning, after natural cooling, obtains the presoma of reaction product;
Step 4: calcining: the presoma that step 3 is obtained is calcined at 1000 DEG C in crucible after grinding uniformly, And 180min is kept the temperature, then cooled to room temperature, obtains the high near infrared reflectivity blue pigment.
Comparative example 1.
A kind of preparation method of blue near-infrared reflection pigment is provided, comprising the following steps:
(1) cabaltous nitrate hexahydrate, ANN aluminium nitrate nonahydrate being weighed according to stoichiometric ratio, dissolved organic matter is glycine, It introduces, above-mentioned raw materials and dissolved organic matter is dissolved in deionized water, mixing time is by the 100% of its stoichiometric ratio 30min obtains the solution of stable uniform.
(2) the uniform solution of aforementioned stable is placed in electric furnace the spontaneous combustion at a temperature of 350 DEG C, is kept the temperature after burning 20min, natural cooling obtain the presoma of reaction product.
(3) it by above-mentioned presoma, is ground uniformly with agate, in crucible, is calcined at 900 DEG C, keep the temperature 80min, from It is so cooled to room temperature, obtains blue near-infrared reflection pigment.
Experiment test:
It will be made from high near infrared reflectivity blue pigment made from above-described embodiment 1 to embodiment 4 and comparative example 1 Blue near-infrared reflection pigment uses color difference meter and near infrared reflectivity instrument to detect respectively, and the results are shown in Table 1.
The blue face of high near infrared reflectivity blue pigment and comparative example 1 made from 1 embodiment 1 to embodiment 4 of table
The performance indicator contrast table of material
Embodiment The molar ratio of titanium ion and cobalt ions Penetrate the Lab value of pigment The reflectivity (%) of pigment
Comparative example 1 / L*=32.3, a*=+5.2, b*=-42.4 45.5
Embodiment 1 0.2 ︰ 1 L*=34.7, a*=+5.5, b*=-40.1 52.2
Embodiment 2 0.5 ︰ 1 L*=36.2, a*=+5.7, b*=-38.5 57.3
Embodiment 3 1.5 ︰ 1 L*=38.6, a*=+6.1, b*=-34.4 63.1
Embodiment 4 3 ︰ 1 L*=41.4, a*=+6.5, b*=-30.7 69.7
As above-mentioned comparative experiments it is found that high near infrared reflectivity blue pigment made from the application is made relative to comparative example 1 Blue near-infrared reflection pigment have better color development ability and reflectivity, in addition, the present invention can by adjusting titanium from Son, it can be achieved that the shade to colorant regulates and controls, can be prepared and be of different shades (by light blue with cobalt ions molar ratio To dark blue) high near infrared reflectivity blue pigment.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than the present invention is protected The limitation of range is protected, although explaining in detail referring to preferred embodiment to the present invention, those skilled in the art are answered Work as understanding, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the reality of technical solution of the present invention Matter and range.

Claims (9)

1. a kind of preparation method of high near infrared reflectivity blue pigment, it is characterised in that: it the following steps are included:
Step 1: the first suspension of preparation: it is soluble in water with certain mass percent by polyvinylpyrrolidone, and use magnetic Power blender stirs certain time, the first solution is obtained, then by rutile titanium dioxide powder with certain quality percentage Number is added in the first solution, and after a certain period of time with magnetic stirrer, moves on to ultrasonic disperser ultrasound certain time, Form the first suspension of stable uniform;
Step 2: the second suspension of preparation: weighing cabaltous nitrate hexahydrate and ANN aluminium nitrate nonahydrate as oxygen according to stoichiometric ratio Agent weighs dissolved organic matter as reducing agent, then by cabaltous nitrate hexahydrate, ANN aluminium nitrate nonahydrate and dissolved organic matter It is dissolved in the first suspension that step 1 obtains, is stirred, the second suspension of stable uniform is made;
Step 3: combustion reaction: the second suspension made from step 2 being placed in electric furnace the spontaneous combustion under certain temperature, is fired Held for some time after burning after natural cooling, obtains the presoma of reaction product;
Step 4: calcining: the presoma that step 3 is obtained is calcined under certain temperature after grinding uniformly, and keeps the temperature a timing Between, then cooled to room temperature, obtains the high near infrared reflectivity blue pigment.
2. a kind of preparation method of high near infrared reflectivity blue pigment according to claim 1, it is characterised in that: described In step 1, polyvinylpyrrolidone is dissolved in deionized water with mass percent for 1%~6%, and use magnetic stirring apparatus 15min~30min is stirred, the first solution is obtained.
3. a kind of preparation method of high near infrared reflectivity blue pigment according to claim 1, it is characterised in that: described In step 1, then rutile titanium dioxide powder is added in the first solution with mass percent for 2%~45%, and After magnetic stirrer 15min~40min, ultrasonic disperser ultrasound 15min~45min is moved on to, forms stable uniform The first suspension.
4. a kind of preparation method of high near infrared reflectivity blue pigment according to claim 1, it is characterised in that: described In step 2, the dissolved organic matter is one of glycine, Beta-alanine, urea, sucrose or citric acid.
5. a kind of preparation method of high near infrared reflectivity blue pigment according to claim 1, it is characterised in that: described In step 2, in second suspension, the molar ratio of titanium ion and cobalt ions is 0.2~5 ︰ 1.
6. a kind of preparation method of high near infrared reflectivity blue pigment according to claim 1, it is characterised in that: described In step 2, the time of the stirring is 30min~60min.
7. a kind of preparation method of high near infrared reflectivity blue pigment according to claim 1, it is characterised in that: described In step 3, the second suspension made from step 2 is placed in electric furnace the spontaneous combustion at 300 DEG C~500 DEG C, is protected after burning Warm 10min~60min after natural cooling, obtains the presoma of reaction product.
8. a kind of preparation method of high near infrared reflectivity blue pigment according to claim 1, it is characterised in that: described In step 4, the presoma that step 3 is obtained, grinding uniformly after, calcined at 900 DEG C~1100 DEG C, and keep the temperature 60min~ 210min, then cooled to room temperature, obtains the high near infrared reflectivity blue pigment.
9. a kind of high near infrared reflectivity blue pigment, it is characterised in that: be one kind described in claim 1 to 8 any one High near infrared reflectivity blue pigment obtained by the preparation method of high near infrared reflectivity blue pigment.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112441623A (en) * 2020-11-17 2021-03-05 浙大宁波理工学院 Preparation of high near-infrared reflection color pigment by using modified cobalt blue pigment

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