CN107629782B - Preparation method of tungsten oxide-mica photochromic pearlescent pigment and dispersion liquid thereof - Google Patents
Preparation method of tungsten oxide-mica photochromic pearlescent pigment and dispersion liquid thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a tungsten oxide-mica photochromic pearlescent pigment and a dispersion liquid thereof, belonging to the field of preparation of novel functional materials. In order to overcome the defects of the prior art, the invention uniformly coats the tungsten oxide on the surface of the mica by the aid of water-soluble organic matters and the adjustment of pH, thereby preparing the tungsten oxide-mica photochromic pearlescent pigment. The obtained powder or dispersion liquid thereof is directly placed under an ultraviolet lamp to be irradiated for different time to observe the photochromic effect, and the prepared powder and dispersion liquid show good photochromic effect under the irradiation of the ultraviolet lamp, and have high photoresponse speed and good photochromic reversibility. The method is a low-temperature chemical synthesis method, is mild, simple, efficient and easy for industrial amplification.
Description
Technical Field
The invention belongs to the field of preparation of novel functional materials, and relates to a preparation method and application of a tungsten oxide-mica photochromic pearlescent pigment and a dispersion liquid thereof.
Background
Pearlescent pigments, as a pigment composed of mica coated with a thin layer of metal oxide, have been widely used in the fields of architectural decoration, inks, automotive paints, textile printing, and the like because of their excellent chemical and high temperature resistance. Pearlescent pigment (MO)x-mica: MO (metal oxide semiconductor)xGenerally referred to as transition metal oxide) has the advantages of good stability and long service life, and can greatly improve the additional value of common transition metal oxides. MO (metal oxide semiconductor)xThe magic color and the various functions of the mica-based pigment pearlescent pigment provide a brand new color system and color quality for products and have huge market share in the world. To date, titanium oxide (TiO) is a well-established pearlescent pigment2) Tin oxide (SnO)2) Iron oxide (Fe)2O3) Mica pearlescent pigments.
The existing tungsten oxide photoluminescence materials generally have the problems of slow photoresponse, low photochromic efficiency, poor reversibility, necessity of an ultraviolet light source and the like, which greatly influences the practical application prospect. In order to further improve the optical properties (reflectivity, absorption, scattering, etc.) of mica-based pearlescent pigments, the choice of the oxide compounded with mica is critical. Tungsten oxide has been widely used in the fields of catalysis, optical and electrical devices, such as photocatalysts, gas sensing, smart windows, etc., because of its low toxicity, high reactivity and good resistance to photo-corrosion. More importantly, tungsten oxide has excellent coloring effect, is one of the most widely used coloring materials at present, and can be applied to electrochromic devices, gasochromic devices and photochromic devices. In addition, tungsten oxide has excellent physicochemical properties, and is widely used in the fields of catalysis, sensing and photoelectricity, such as water decomposition, catalytic degradation of pollutants, supercapacitors, electrochromic devices and the like.
However, there are few reports on tungsten oxide-mica photochromic pearlescent pigments. So far, no report of growing a tungsten oxide structure on the surface of micron-sized mica and researching the photochromic effect of the tungsten oxide structure is found in the prior art.
Disclosure of Invention
In order to overcome the defects in the application of tungsten oxide photoluminescent materials in the prior art, the invention provides a preparation method of a tungsten oxide-mica photochromic pearlescent pigment. The invention adopts a low-temperature chemical synthesis method to uniformly and completely coat tungsten oxide on the surface of a micron-sized mica substrate to obtain a tungsten oxide-mica powder material, and the powder material is further dispersed in an aqueous solution to obtain a tungsten oxide-mica dispersion liquid. The preparation method provided by the invention is simple and controllable, easy to amplify and strong in industrial feasibility, and the prepared pigment can realize a high-efficiency, rapid and reversible photochromic effect under the irradiation of an ultraviolet lamp.
The invention realizes the technical effects through the following technical scheme:
the invention provides a preparation method of a tungsten oxide-mica photochromic pearlescent pigment, which comprises the following steps:
1) weighing soluble tungstate, adding the soluble tungstate into deionized water, and stirring for 50-70 minutes under the condition of 400-1500 rpm to obtain an aqueous solution of tungstate, wherein the molar concentration of the aqueous solution of tungstate is 0.001-1.0M;
2) adding a micron-sized mica substrate into a tungstate aqueous solution, and stirring for 25-35 minutes under the condition of 400-1500 rpm to obtain a suspension A, wherein the molar concentration of the mica substrate in the suspension A is 0.001-1.0M;
3) weighing a water-soluble organic matter, adding the water-soluble organic matter into the suspension A, and stirring for 2-26 hours under the condition of 400-800 rpm to obtain a suspension B, wherein the molar concentration of the water-soluble organic matter in the suspension B is 0.005-0.100M;
4) slowly adding inorganic acid into the suspension B dropwise under the stirring state, and adjusting the pH value of the suspension B to 0.1-2; stirring is continued for 4 hours under the condition of 400-800 r/M to obtain a suspension C, and the molar concentration of the inorganic acid in the suspension C is 0.010-5.0M;
5) after the reaction is finished, centrifuging the suspension C for solid-liquid separation, collecting lower-layer solid, adding the lower-layer solid into alcohol for ultrasonic cleaning, centrifuging and collecting the lower-layer solid, and repeating the operation for 3-5 times; ultrasonically cleaning the substrate for 1 time by using deionized water, centrifugally collecting lower-layer solids, and drying the product in a constant-temperature environment to obtain the tungsten oxide-mica photochromic pearlescent pigment.
The soluble tungstate in the preparation method is any salt containing tungsten, and preferably, the soluble tungstate is one of sodium tungstate and ammonium tungstate.
After the aqueous solution of tungstate is obtained in the preparation method, the method also comprises the step of adding doping elements into the aqueous solution of tungstate; preferably, the doping element is one or more of zirconium, aluminum, copper, titanium, molybdenum or lithium; the method for adding the doping element is to directly add the aqueous solution prepared by doping element salts into the aqueous solution of tungstate, wherein the amount of the doping element substances is 0.1-20% of that of the tungsten element substances; the addition of the doping element can change the photochromic light response range of the tungsten oxide, improve the light response and the photochromic reversibility, so that the composite powder has better photochromic effect.
In the preparation method, the micron-sized mica substrate in the step 2) is a mica substrate or an oxide modified mica substrate, and is preferably a titanium oxide modified mica substrate.
In the preparation method, the water-soluble organic substance in the step 3) is one, two or more of polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), polyethylene glycol (PEG), Cetyl Trimethyl Ammonium Bromide (CTAB) or Sodium Dodecyl Benzene Sulfonate (SDBS).
In the preparation method, the inorganic acid in the step 4) is one or more of hydrochloric acid, nitric acid or sulfuric acid; taking hydrochloric acid as an example, the acid is obtained by diluting concentrated hydrochloric acid with deionized water, and the concentration of the concentrated hydrochloric acid is 20-38%; the concentration of the acid obtained after the concentrated hydrochloric acid is diluted is 0.5-5M, and the final concentration of the hydrochloric acid in the suspension C is 0.010-5.0M.
In the preparation method, the acid diluted by the deionized water in the step 4) is added dropwise and slowly, and the total dropwise adding time is not less than 30 minutes;
a preparation method of a mica photochromic pearlescent pigment dispersion liquid modified by tungsten oxide-titanium oxide specifically comprises the following steps:
adding the tungsten oxide-mica photochromic pearlescent pigment into 1-10 wt% of polyvinylpyrrolidone aqueous solution, and stirring the mixture under the condition of 400-2500 rpm to uniformly disperse the mixture, wherein the obtained viscous solution is the dispersion liquid of the tungsten oxide-mica photochromic pearlescent pigment, and the dispersion liquid can be used as slurry for a subsequent coating process. Preferably, the molecular weight of the polyvinylpyrrolidone is between 5000-;
the invention also claims an application, namely the application of the tungsten oxide-mica photochromic pearlescent pigment in preparing the photochromic luminescent pigment. The tungsten oxide-mica powder material obtained by the invention has excellent photochromic effect, can show photochromic reaction within a few minutes of ultraviolet lamp irradiation, and is far superior to the traditional tungsten oxide powder. Meanwhile, the photochromic reversibility is good, and the primary color can be recovered within a short time (several minutes to dozens of minutes) after the ultraviolet lamp is removed.
The observation of the photochromic effect is that the mica powder modified by tungsten oxide-titanium oxide or the mica water dispersion liquid modified by tungsten oxide-titanium oxide is directly placed under an ultraviolet lamp to be irradiated for different time, the observation of the fading process is that the mica powder modified by tungsten oxide-titanium oxide or the mica dispersion liquid modified by tungsten oxide-titanium oxide is removed from the ultraviolet lamp to be irradiated, and the reversibility of the photochromic process is realized by repeating the processes of irradiation, removal and irradiation of the ultraviolet lamp. Wherein the irradiation time of the ultraviolet lamp is 1-60 minutes, preferably 3-30 minutes;
the invention provides a preparation method of a tungsten oxide-mica photochromic pearlescent pigment and a dispersion liquid thereof, and a method for preparing the tungsten oxide-mica powder into the dispersion liquid based on the preparation method.
According to the invention, the water-soluble polymer is added, so that the tungsten oxide is successfully coated on the surface of the mica, and the composite product has a good photochromic effect due to the addition of the water-soluble polymer. Under the irradiation of an ultraviolet lamp, the high-efficiency, quick and reversible photochromism is realized. Compared with the prior art, the invention has the following innovations and advantages:
1. the invention organically combines the photochromic material with the traditional pigment to finally synthesize and prepare the micron-sized tungsten oxide-mica photochromic pearlescent pigment, and prepares the dispersion liquid which can be coated on different application surfaces on the basis of the micron-sized tungsten oxide-mica photochromic pearlescent pigment.
2. In the tungsten oxide-mica powder product raw materials prepared by the method, the mica has good stability and low price, and the combination of the tungsten oxide and the mica can provide a good carrier for the application of the tungsten oxide photochromic material while improving the additional value of the traditional pigment, so that the method has bright commercial prospect.
3. The addition of the water-soluble polymer in the preparation method not only ensures the complete coating of the tungsten oxide on the surface of the mica, but also plays a key role in improving the photochromic effect of the complex.
4. The preparation method of the tungsten oxide-mica composite powder adopts a wet chemical synthesis method, the whole process is completed under the room temperature condition, the complex equipment and higher energy consumption cost are avoided, the reaction condition is mild, the operation is convenient, and the method is suitable for industrial production.
5. The preparation method adopted by the invention can realize the complete coating of the tungsten oxide on the micron-sized mica substrate, and the obtained tungsten oxide-mica composite powder has excellent photochromic effect, can show photochromic reaction within a few minutes of ultraviolet lamp irradiation, and is far superior to the traditional tungsten oxide powder. Meanwhile, the photochromic reversibility is good, and the primary color can be recovered in a short time after the ultraviolet lamp is removed.
Drawings
FIG. 1 is a scanning electron micrograph of a mica photochromic pearlescent pigment modified by tungsten oxide-titanium oxide: the left image is a photograph of tungsten oxide particles coated on mica sheets with high resolution, and the right image is a photograph of tungsten oxide particles coated on mica sheets with low resolution.
FIG. 2 is an elemental analysis chart of a mica photochromic pearlescent pigment modified by tungsten oxide-titanium oxide.
FIG. 3 is a photochromic diagram of a mica photochromic pearlescent pigment modified by tungsten oxide-titanium oxide under the irradiation of an ultraviolet lamp.
FIG. 4 is a diagram of the photochromic effect of the dispersion prepared by the mica photochromic pearlescent pigment modified by tungsten oxide-titanium oxide.
FIG. 5 is a graph of the photochromic effect of a mica photochromic pearlescent pigment modified with zirconium-doped tungsten oxide-titanium oxide.
Detailed Description
The invention is further illustrated in the following description with reference to the figures and the specific examples, which are intended to illustrate the invention only and not to show the scope of protection of the invention, which is defined in any way by the claims. The technical solutions obtained by modifying or replacing the present invention by those skilled in the art without creative efforts are included in the patent protection scope of the present invention.
Experimental example 1 preparation of tungsten oxide-titanium oxide modified mica photochromic pearlescent pigment and dispersion liquid of the present invention
1.1 preparation of tungsten oxide-titanium oxide modified mica photochromic pearlescent pigments
0.5g of sodium tungstate is added into 30ml of deionized water, and the mixture is stirred for 1 to 3 hours at the rotating speed of 1000 revolutions per minute until the sodium tungstate is completely dissolved to obtain a solution. 0.6g of the titanium oxide-coated mica substrate was weighed into the solution, stirred at 1000 rpm for 30 minutes to obtain suspension A, and 0.15g of PVP (polyvinylpyrrolidone) was added thereto, and stirred at 800 rpm for 24 hours to obtain suspension B. Diluting 30% concentrated hydrochloric acid to 2M with deionized water, slowly adding 3ml of 2M hydrochloric acid into the suspension B within 1 hour, and finally continuously stirring and reacting at normal temperature for 1-6 hours. And after the reaction is finished, separating the solution by using a centrifugal machine, collecting lower-layer solid, ultrasonically cleaning and centrifuging by using 40ml of alcohol, collecting the lower-layer solid after each centrifugation, repeating the step for 5 times, ultrasonically cleaning for 1 time by using deionized water, centrifugally collecting the lower-layer solid, and drying the product in a constant-temperature oven at the temperature of 60 ℃ to obtain the tungsten oxide-titanium oxide modified mica photochromic pearlescent pigment.
1.2 preparation of a tungsten oxide-titanium oxide-coated mica photochromic pearlescent pigment Dispersion
3g of PVP (molecular weight of 50000) is added into 50ml of water, after stirring for 30 minutes, 0.5g of tungsten oxide-titanium oxide-mica photochromic pearlescent pigment is weighed and added, and stirring is continued for 3 hours to obtain uniform dispersion for later use.
1.3 photochromic of tungsten oxide-titanium oxide coated mica pearlescent pigments
The tungsten oxide-mica photochromic pearlescent pigment obtained by the preparation method is characterized by X-ray diffraction and element analysis means. FIG. 1 is a scanning electron microscope image of a mica photochromic pearlescent pigment modified by tungsten oxide-titanium oxide of the present invention; it can be seen from the figure that the tungsten oxide-titanium oxide is well coated on the surface of the mica substrate.
FIG. 2 is an elemental analysis chart of the tungsten oxide-titanium oxide modified mica photochromic pearlescent pigment of the present invention. The graph shows that the content of Ti in the photochromic pearlescent pigment is 25.85 percent, and the content of W element is 6.85 percent, which indicates that the tungsten oxide-titanium oxide is coated on the mica substrate.
And analyzing the optical absorption characteristics of the powder by using an ultraviolet-visible spectrum. And (5) observing the growth condition of the tungsten oxide on the surface of the mica by using a scanning electron microscope photo. And placing the mica composite powder modified by the tungsten oxide-titanium oxide under an ultraviolet lamp for 3 minutes, observing the color change, taking out the mica composite powder, recording the color change, removing the ultraviolet lamp for irradiation, placing the mica composite powder at room temperature for 1 minute to 24 hours, and recording the color change. After the color is changed completely, the ultraviolet lamp is repeatedly irradiated, and the color change is observed. FIG. 3 shows the photochromic effect of the mica photochromic pearl pigment modified by tungsten oxide-titanium oxide under the irradiation of an ultraviolet lamp. It can be seen from the figure that the tungsten oxide-titanium oxide modified mica photochromic pearlescent pigment is initially pale yellow, appears dark blue after being irradiated for 3 minutes by the ultraviolet lamp, and the pigment is substantially restored to the initial color after the ultraviolet lamp is removed for 16 hours.
And (3) placing the slurry prepared from the mica photochromic pearlescent pigment modified by tungsten oxide-titanium oxide under an ultraviolet lamp for 10 seconds to 3 minutes, observing the color change, taking out the slurry for recording the color change, and placing the slurry at room temperature for 1 to 30 minutes after the ultraviolet lamp is removed for irradiation, and recording the color change. After the color is changed completely, the ultraviolet lamp is repeatedly irradiated, and the color change is observed. FIG. 4 shows the photochromic effect of the dispersion prepared by the mica photochromic pearlescent pigment modified by tungsten oxide-titanium oxide under the irradiation of an ultraviolet lamp. The dispersion liquid shows better photochromic effect under the irradiation of an ultraviolet lamp. The initial color of the dispersion liquid is light yellow turbid liquid, bright blue is presented after the ultraviolet lamp irradiates for 10 seconds, most of blue is removed after the ultraviolet lamp is removed and placed for 1 minute, and the blue is completely removed after the ultraviolet lamp is placed for 5 minutes, and the initial color is recovered.
Experimental example 2 preparation of zirconium ion-doped tungsten oxide-titanium oxide-modified mica photochromic pearlescent pigment and dispersion liquid of the present invention
2.1 preparation of zirconium-doped tungsten oxide-titanium oxide-modified mica photochromic pearlescent pigments
0.7g of sodium tungstate and 0.005g of zirconium chloride are added into 30ml of deionized water, and the mixture is stirred for 1 hour at the rotating speed of 1000 rpm until the sodium tungstate and the zirconium chloride are completely dissolved to obtain a solution. 0.8g of the titanium oxide-coated mica substrate was weighed out and added to the solution, and after stirring at 1000 rpm for 30 minutes, suspension A was obtained, and after adding 0.10g of PVP thereto, suspension B was obtained after stirring at 800 rpm for 24 hours. 4ml of 2M hydrochloric acid was added dropwise to the suspension B over 1 hour, and the reaction was continued for 3 hours with stirring at room temperature. After the reaction was complete, the solution was layered with a centrifuge, the lower layer of solids was collected, ultrasonically washed with 40ml of alcohol and centrifuged, after each centrifugation, the lower layer of solids was collected, the procedure was repeated 5 times, then ultrasonically washed with deionized water 1 time and centrifuged to collect the lower layer of solids. And then putting the product into a constant temperature environment of 60 ℃ for drying for 2 hours.
2.2 preparation of zirconium-doped tungsten oxide-titanium oxide-modified mica photochromic pearlescent pigment Dispersion
2g of PVP (molecular weight of 360000) is added into 50ml of water, after stirring for 30 minutes, 0.3g of zirconium-doped tungsten oxide-titanium oxide-mica composite powder is weighed and added, and stirring is continued for 3 hours to obtain uniform dispersion liquid for later use.
2.3 photochromic Effect of zirconium-doped tungsten oxide-titanium oxide-modified mica photochromic pearlescent pigments and dispersions
The zirconium-doped tungsten oxide-titanium oxide modified mica photochromic pearlescent pigment is placed under an ultraviolet lamp for 3 minutes, and then the color change is observed, and the result is shown in figure 5. After the irradiation of the ultraviolet lamp is removed, the mixture is placed at room temperature for 1 minute to 24 hours, and the color change is recorded. After the color is changed completely, the ultraviolet lamp is repeatedly irradiated, and the color change is observed. FIG. 5 shows the photochromic effect of the zirconium-doped tungsten oxide-titanium oxide modified mica photochromic pearlescent pigment under the irradiation of an ultraviolet lamp. The initial color of the prepared powder is light yellow, the powder can show dark blue after being illuminated under an ultraviolet lamp for 3 minutes, compared with an undoped sample, the color change of the zirconium-doped sample is more obvious, and the influence of ion doping on the photochromic effect of the sample is highlighted.
And (3) placing the dispersion prepared from the zirconium-doped tungsten oxide-titanium oxide modified mica photochromic pearlescent pigment under an ultraviolet lamp for 10 seconds to 3 minutes, observing the color change, taking out and recording the color change, and placing at room temperature for 1 to 30 minutes after the ultraviolet lamp is removed for irradiation, and recording the color change. After the color is changed completely, the ultraviolet lamp is repeatedly irradiated, and the color change is observed. The color change is close to that of fig. 4.
Claims (5)
1. A preparation method of tungsten oxide-mica photochromic pearlescent pigment specifically comprises the following steps:
1) weighing soluble tungstate, adding the soluble tungstate into deionized water, and stirring for 50-70 minutes under the condition of 400-1500 rpm to obtain an aqueous solution of tungstate, wherein the molar concentration of the aqueous solution of tungstate is 0.001-1.0M;
2) adding a micron-sized mica substrate into a tungstate aqueous solution, and stirring for 25-35 minutes under the condition of 400-1500 rpm to obtain a suspension A, wherein the molar concentration of the mica substrate in the suspension A is 0.001-1.0M;
3) weighing a water-soluble organic matter, adding the water-soluble organic matter into the suspension A, and stirring for 2-26 hours under the condition of 400-800 rpm to obtain a suspension B, wherein the molar concentration of the water-soluble organic matter in the suspension B is 0.005-0.100M;
4) slowly adding inorganic acid into the suspension B dropwise under the stirring state, and adjusting the pH value of the suspension B to 0.1-2; stirring is continued for 4 hours under the condition of 400-800 r/M to obtain a suspension C, and the molar concentration of the inorganic acid in the suspension C is 0.010-5.0M;
5) after the reaction is finished, centrifuging the suspension C for solid-liquid separation, collecting lower-layer solid, adding the lower-layer solid into alcohol for ultrasonic cleaning, centrifuging and collecting the lower-layer solid, and repeating the operation for 3-5 times; ultrasonically cleaning for 1 time by using deionized water, centrifugally collecting lower-layer solids, and drying a product in a constant-temperature environment to obtain the tungsten oxide-mica photochromic pearlescent pigment;
the method for adding the doping element comprises the steps of directly adding an aqueous solution prepared by doping element salts into the aqueous solution of the tungstate, wherein the amount of the doping element substances is 0.1-20% of that of the tungsten element substances;
the water-soluble organic matter is polyvinylpyrrolidone;
the micron-sized mica substrate is a titanium oxide modified mica substrate.
2. The method for preparing the tungsten oxide-mica photochromic pearlescent pigment of claim 1, wherein the soluble tungstate is one or more of sodium tungstate and ammonium tungstate.
3. The method for preparing the tungsten oxide-mica photochromic pearlescent pigment according to claim 1, wherein the inorganic acid is one or more of hydrochloric acid, nitric acid or sulfuric acid.
4. A preparation method of a mica photochromic pearlescent pigment dispersion liquid modified by tungsten oxide-titanium oxide is characterized by comprising the following steps:
the mica photochromic pearlescent pigment modified by tungsten oxide-titanium oxide prepared by the preparation method of claim 1 is added into 1-10 wt% of polyvinylpyrrolidone aqueous solution and stirred to be uniformly dispersed under the condition of 400-2500 rpm, and the obtained viscous solution is the mica photochromic pearlescent pigment dispersion liquid modified by tungsten oxide-titanium oxide.
5. The method for preparing the tungsten oxide-titanium oxide modified mica photochromic pearlescent pigment dispersion liquid as claimed in claim 4, wherein the molecular weight of the polyvinylpyrrolidone is between 5000-360000.
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