CN113024853B - Preparation method of high-transmittance infrared-blocking polycarbonate color master batch - Google Patents
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Abstract
The invention provides a preparation method of a high-transmittance infrared-blocking polycarbonate color master batch, which comprises the steps of dissolving stannous salt in strong acid, slowly adding a very small amount of tin powder in the stirring process, and adding carbonate until no bubbles are generated to obtain turbid liquid; adding indium salt, cesium salt and hydrogen peroxide into the suspension, stirring, washing and drying to obtain powder; pressing the powder into a rod shape by using uniaxial pressure and cold isostatic pressing, heating in a current field of 15-25V/cm, carrying out temperature programming until the limiting current is 0.8-8A, keeping at 200-240 ℃ for 6-12 min, and stopping electrifying to obtain indium-cesium co-doped tin oxide; mixing indium-cesium co-doped tin oxide with polycarbonate and lubricant paraffin, adding auxiliary materials including rhenium heptoxide, an organic phosphorus flame retardant, tea polyphenol and rosin resin, uniformly mixing, adding into a double-screw extruder, extruding, cooling, drawing, air-drying and granulating to obtain the high-transmittance infrared blocking polycarbonate color master batch. The master batch can absorb sunlight in an infrared band after being stretched and formed at a high temperature, has a heat insulation and sun protection function, and has an infrared blocking rate of more than 97% at a wavelength of 950 nm.
Description
Technical Field
The invention relates to a high-transmittance infrared-blocking polycarbonate color master batch and a preparation method thereof, belonging to the field of infrared-blocking materials.
Background
The color master batch is a common plastic colorant and has the following advantages: 1. the pigment has better dispersibility in products; 2. the chemical stability of the pigment is favorably kept; 3. the color stability of the product is ensured; 4. the health of operators is protected; 5. the environment is kept clean, and vessels are not polluted; 6. simple process, easy color conversion, and saved time and raw materials.
Infrared light has an obvious thermal effect, which easily causes the ambient temperature to rise, and heat insulation materials are needed to achieve the effect of heat insulation and energy saving. In recent years, tin oxide attracts people to pay attention due to excellent photoelectric properties, and tin oxide doped with indium and cesium has extremely strong absorption characteristics in an infrared region and high visible light transmittance, so that the tin oxide has wide application prospects in the aspects of infrared blocking, heat insulation and the like. Indium and cesium co-doped tin oxide, polycarbonate and the like are melted and mixed to prepare the polycarbonate color master batch with infrared barrier, and the polycarbonate color master batch can be applied to the field of heat insulation and energy saving.
The indium-cesium co-doped tin oxide prepared by the traditional method has the infrared blocking rate of not more than 90%, and cesium hydroxide is used in part of process raw materials, so that the cost is high, the stability is poor, and the indium-cesium co-doped tin oxide is harmful to human bodies and the environment. Therefore, the preparation method of the high-transmittance infrared-blocking polycarbonate color master batch can enable indium and cesium to better replace partial tin, realize reasonable lattice doping, greatly shorten the phase forming temperature and time of the indium-cesium co-doped tin oxide material on one hand, and improve the capacity of the tin-oxygen bond to absorb near-infrared light with specific wavelength by the indium-oxygen bond and the cesium-oxygen bond on the other hand, so that the capacity of the doped product to block near-infrared light can be improved, and the problems in the content can be solved.
Disclosure of Invention
The invention aims to provide a preparation method of a high-transmittance infrared-blocking polycarbonate color master batch. Compared with the traditional sintering technology, the technology greatly reduces the phase forming temperature and the calcining time, has better crystallinity and larger area, and can further improve the infrared blocking capability; secondly, a dispersing agent is not needed, a lubricating agent is added in a controlled manner, so that the indium-cesium co-doped tin oxide powder, the polycarbonate and other components are uniformly mixed, and finally the high-infrared-transmission barrier polycarbonate color master batch is prepared by melt blending through a double-screw extruder.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a high-transmittance infrared-blocking polycarbonate color master batch comprises the following steps,
1) dissolving 2-valent stannous salt in a strong acid solution with the concentration of 2M, slowly adding a very small amount of tin powder in the magnetic stirring process, and then adding solid weak base carbonate, wherein the molar weight ratio of the stannous salt to the carbonate to the tin powder is 1: 1: 0.005, magnetically stirring for 1-3 h until no bubbles are generated in the reaction, and obtaining suspension A;
2) adding indium salt, cesium salt and hydrogen peroxide into the suspension A to ensure that the tin salt, the indium salt, the cesium salt and the hydrogen peroxide meet the molar stoichiometric ratio (1-x-y): x: y: (1-x-y) (x is more than 0 and less than 1, y is more than 0 and less than 1), magnetically stirring for 2-4 h, and washing for 2-3 times by using deionized water and absolute ethyl alcohol; drying the mixture in a blast oven at the temperature of 60-80 ℃ for 12-18 h to obtain powder B;
3) pressing the powder B into a rod-shaped precursor by using a uniaxial pressure of 4MPa and a cold isostatic pressure of 300MPa, reserving a hole at each of two ends for connecting a platinum wire, connecting and suspending the rod-shaped object in the middle of a muffle furnace by using the platinum wire, heating the rod-shaped object in a current field of 15-25V/cm, programming the temperature until a limited current of 0.8-8A is reached, keeping the temperature at 200-240 ℃ for 6-12 min, and stopping electrifying to obtain a final product, namely indium and cesium co-doped tin oxide;
4) grinding the indium-cesium co-doped tin oxide into powder, mixing the powder with polycarbonate and lubricant paraffin, wherein the components in parts by weight are 35 parts, 60 parts and 5 parts respectively, meanwhile, adding 3 parts of rhenium heptoxide serving as other auxiliary materials, 10 parts of an organic phosphorus flame retardant, 6 parts of tea polyphenol and 6 parts of rosin resin, uniformly mixing, adding into a double-screw extruder, heating at nine sections, extruding, cooling, drawing strips, air-drying and granulating to obtain the high-transmittance infrared blocking polycarbonate color master batch.
Preferably, in the step 1), the stannous salt is one or a combination of stannous chloride and stannous sulfate; the strong acid is one or the combination of hydrochloric acid or sulfuric acid; the carbonate is one or the combination of sodium carbonate, potassium carbonate or lithium carbonate.
Preferably, in the step 2), the indium salt is one or a combination of indium chloride and indium sulfate; the cesium salt is one or a combination of cesium chloride or cesium sulfate.
Preferably, in the step 3), the cross section of the rod-shaped precursor is 3mm × 2.1mm, and the length is 20 mm; the temperature programming rate is 10-15 ℃/min.
Preferably, in the step 4), the nine-stage processing temperature of the twin-screw extruder is set as follows: the temperature in the first zone is 130 ℃, the temperature in the second zone is 185 ℃, the temperature in the third zone is 238 ℃, the temperature in the fourth zone is 250 ℃, the temperature in the fifth zone is 260 ℃, the temperature in the sixth zone is 260 ℃, the temperature in the seventh zone is 255 ℃, the temperature in the eighth zone is 230 ℃ and the temperature in the ninth zone is 180 ℃.
Compared with the prior art, the invention has the following beneficial effects:
the invention aims to provide a preparation method of a high-transmittance infrared-blocking polycarbonate color master batch. Compared with the traditional sintering technology:
1) the temperature of the crystal material phase formation and the calcination time are greatly reduced, and the crystal material has good crystallinity, large specific surface area and excellent infrared blocking capability;
2) a dispersing agent is not needed, a lubricating agent is added in a controlled manner, so that the indium-cesium co-doped tin oxide powder, the polycarbonate and other components are uniformly mixed, and finally the high-transmittance infrared-blocking polycarbonate color master batch is prepared by melt blending through a double-screw extruder.
Drawings
FIG. 1 is an SEM image of indium-cesium co-doped tin oxide powder in example 1
FIG. 2 is a SEM (scanning Electron microscope) cross-section of example 2 showing that indium and cesium are added to co-doped tin oxide high-transmittance infrared-blocking polycarbonate master batch
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
dissolving stannous chloride 2 in hydrochloric acid solution with the concentration of 2M, slowly adding a very small amount of tin powder in the magnetic stirring process, and then adding solid weak base sodium carbonate, wherein the molar weight ratio of the stannous chloride to the sodium carbonate to the tin powder is 1: 1: 0.5, magnetically stirring for 1 hour until no bubbles are generated in the reaction, and obtaining suspension A; adding indium chloride, cesium chloride and hydrogen peroxide into the suspension A to ensure that the molar stoichiometric ratio of tin chloride to indium chloride to cesium chloride to hydrogen peroxide is 1: 0.556: 0.556: 1, magnetically stirring for 2 hours, and washing for 2 times by using deionized water and absolute ethyl alcohol; drying for 12h at 60 ℃ in a blast oven to obtain powder B; pressing the powder B into a rod with the cross section of 3mm multiplied by 2.1mm and the length of 20mm by using a uniaxial pressure of 4MPa and a cold isostatic pressure of 300MPa, reserving a hole at each of two ends for connecting a platinum wire, connecting and suspending the rod in the middle of a muffle furnace by using the platinum wire, heating the rod in a current field of 20V/cm, heating the rod at a heating rate of 15 ℃/min until reaching a limited current of 4A, keeping the temperature at 200 ℃ for 12min, and stopping electrifying to obtain a final product, namely the indium-cesium co-doped tin oxide; grinding the indium-cesium co-doped tin oxide into powder, mixing the powder with polycarbonate and lubricant paraffin, wherein the components in parts by weight are 35 parts, 60 parts and 5 parts respectively, and adding 3 parts of rhenium heptoxide serving as other auxiliary materials, 10 parts of an organic phosphorus flame retardant, 6 parts of tea polyphenol and 6 parts of rosin resin, uniformly mixing, adding the mixture into a double-screw extruder, and controlling the processing temperature of the double-screw extruder: the temperature of the first zone is 130 ℃, the temperature of the second zone is 185 ℃, the temperature of the third zone is 238 ℃, the temperature of the fourth zone is 250 ℃, the temperature of the fifth zone is 260 ℃, the temperature of the sixth zone is 260 ℃, the temperature of the seventh zone is 255 ℃, the temperature of the eighth zone is 230 ℃, the temperature of the ninth zone is 180 ℃, and the high-transmittance infrared-blocking polycarbonate color master batch is prepared by extrusion, cooling, drawing, air-drying and grain-cutting.
Wherein, FIG. 1 is an SEM image of the indium-cesium co-doped tin oxide powder, and the particle size of the powder is 50-100 nm.
The infrared blocking rate of the high infrared transmission blocking polycarbonate 1mm sample wafer added with the indium-cesium co-doped tin oxide was measured, and the results are shown in table 2.
Example two:
dissolving stannous sulfate 2 in a sulfuric acid solution with the concentration of 2M, slowly adding a very small amount of tin powder in the magnetic stirring process, and then adding solid weak base potassium carbonate, wherein the molar weight ratio of the stannous sulfate to the potassium carbonate to the tin powder is 1: 1: 0.005, magnetically stirring for 2 hours until no bubbles are generated in the reaction, and obtaining suspension A; adding indium sulfate, cesium sulfate and hydrogen peroxide into the suspension A to ensure that the molar stoichiometric ratio of tin sulfate to indium sulfate to cesium sulfate to hydrogen peroxide is 1: 0.067: 0.044: 1, magnetically stirring for 4 hours, and washing for 3 times by using deionized water and absolute ethyl alcohol; drying for 12h at 80 ℃ in a blast oven to obtain powder B; pressing the powder B into a rod with the cross section of 3mm multiplied by 2.1mm and the length of 20mm by using a uniaxial pressure of 4MPa and a cold isostatic pressure of 300MPa, reserving a hole at each of two ends for connecting a platinum wire, connecting and suspending the rod in the middle of a muffle furnace by using the platinum wire, heating the rod in a current field of 15V/cm, heating the rod at a heating rate of 10 ℃/min until a limited current of 0.8A is reached, keeping the temperature at 200 ℃ for 12min, and stopping electrifying to obtain a final product, namely the indium-cesium co-doped tin oxide; grinding the indium-cesium co-doped tin oxide into powder, mixing the powder with polycarbonate and lubricant paraffin, wherein the components in parts by weight are 35 parts, 60 parts and 5 parts respectively, and adding 3 parts of rhenium heptoxide serving as other auxiliary materials, 10 parts of an organic phosphorus flame retardant, 6 parts of tea polyphenol and 6 parts of rosin resin, uniformly mixing, adding the mixture into a double-screw extruder, and controlling the processing temperature of the double-screw extruder: the temperature of the first zone is 130 ℃, the temperature of the second zone is 185 ℃, the temperature of the third zone is 238 ℃, the temperature of the fourth zone is 250 ℃, the temperature of the fifth zone is 260 ℃, the temperature of the sixth zone is 260 ℃, the temperature of the seventh zone is 255 ℃, the temperature of the eighth zone is 230 ℃, the temperature of the ninth zone is 180 ℃, and the high-transmittance infrared-blocking polycarbonate color master batch is prepared by extrusion, cooling, drawing, air-drying and grain-cutting.
The particle size of the indium-cesium co-doped tin oxide powder was tested and the results are shown in table 1.
The distribution of indium and cesium co-doped tin oxide in the high-infrared-transmission barrier polycarbonate master batch is tested, and the result is shown in figure 2
The infrared blocking rate of the high infrared transmission blocking polycarbonate 1mm sample wafer added with the indium-cesium co-doped tin oxide was measured, and the results are shown in table 2.
Example three:
dissolving stannous chloride 2 in hydrochloric acid solution with the concentration of 2M, slowly adding a very small amount of tin powder in the magnetic stirring process, and then adding solid weak base lithium carbonate, wherein the molar weight ratio of the stannous chloride, the lithium carbonate and the tin powder is 1: 1: 0.005, magnetically stirring for 2 hours until no bubbles are generated in the reaction, and obtaining suspension A; adding indium chloride, cesium chloride and hydrogen peroxide into the suspension A to ensure that the molar stoichiometric ratio of tin chloride to indium chloride to cesium chloride to hydrogen peroxide is 1: 0.033: 0.078: 1, magnetically stirring for 4 hours, and washing for 3 times by using deionized water and absolute ethyl alcohol; drying for 18h at 60 ℃ in a blast oven to obtain powder B; pressing the powder B into a rod with the cross section of 3mm multiplied by 2.1mm and the length of 20mm by using a uniaxial pressure of 4MPa and a cold isostatic pressure of 300MPa, reserving a hole at each of two ends for connecting a platinum wire, connecting and suspending the rod in the middle of a muffle furnace by using the platinum wire, heating the rod in a current field of 25V/cm, heating the rod at a heating rate of 15 ℃/min until reaching a limited current of 8A, keeping the temperature at 240 ℃ for 6min, and stopping electrifying to obtain a final product, namely the indium-cesium co-doped tin oxide; grinding the indium-cesium co-doped tin oxide into powder, mixing the powder with polycarbonate and lubricant paraffin, wherein the components in parts by weight are 35 parts, 60 parts and 5 parts respectively, and adding 3 parts of rhenium heptoxide serving as other auxiliary materials, 10 parts of an organic phosphorus flame retardant, 6 parts of tea polyphenol and 6 parts of rosin resin, uniformly mixing, adding the mixture into a double-screw extruder, and controlling the processing temperature of the double-screw extruder: the temperature of the first zone is 130 ℃, the temperature of the second zone is 185 ℃, the temperature of the third zone is 238 ℃, the temperature of the fourth zone is 250 ℃, the temperature of the fifth zone is 260 ℃, the temperature of the sixth zone is 260 ℃, the temperature of the seventh zone is 255 ℃, the temperature of the eighth zone is 230 ℃, the temperature of the ninth zone is 180 ℃, and the high-transmittance infrared-blocking polycarbonate color master batch is prepared by extrusion, cooling, drawing, air-drying and grain-cutting.
The infrared blocking rate of the high infrared transmission blocking polycarbonate 1mm sample wafer added with the indium-cesium co-doped tin oxide was measured, and the results are shown in table 2.
TABLE 1 particle size of indium-cesium co-doped tin oxide powder
Sample name | d50(nm) | d90(nm) |
Indium-cesium co-doped tin oxide powder | 25 | 60 |
Table 2 comparison of near infrared blocking rate of high-transmittance infrared blocking polycarbonate 1mm sample plate added with indium-cesium co-doped tin oxide
Sample (I) | 950nm near infrared blocking rate |
Example 1 indium cesium co-doped tin oxide | 97.2% |
Example 2 indium cesium co-doped tin oxide | 98.3% |
Example 3 indium cesium co-doped tin oxide | 97.5% |
Claims (5)
1. A preparation method of a high-transmittance infrared-blocking polycarbonate color master batch is characterized by comprising the following steps;
1) dissolving 2-valent stannous salt in a strong acid solution with the concentration of 2M, slowly adding a very small amount of tin powder in the magnetic stirring process, and then adding solid weak base carbonate, wherein the molar weight ratio of the stannous salt to the carbonate to the tin powder is 1: 1: 0.005, magnetically stirring for 1-3 h until no bubbles are generated in the reaction, and obtaining suspension A;
2) adding indium salt, cesium salt and hydrogen peroxide into the suspension A to ensure that the tin salt, the indium salt, the cesium salt and the hydrogen peroxide meet the molar stoichiometric ratio (1-x-y): x: y: (1-x-y) (x is more than 0 and less than 1, y is more than 0 and less than 1), magnetically stirring for 2-4 h, and washing for 2-3 times by using deionized water and absolute ethyl alcohol; drying the mixture in a blast oven at the temperature of 60-80 ℃ for 12-18 h to obtain powder B;
3) pressing the powder B into a rod-shaped precursor by using a uniaxial pressure of 4MPa and a cold isostatic pressure of 300MPa, reserving a hole at each of two ends for connecting a platinum wire, connecting and suspending the rod-shaped object in the middle of a muffle furnace by using the platinum wire, heating the rod-shaped object in a current field of 15-25V/cm, programming the temperature until a limited current of 0.8-8A is reached, keeping the temperature at 200-240 ℃ for 6-12 min, and stopping electrifying to obtain a final product, namely indium and cesium co-doped tin oxide;
4) grinding the indium-cesium co-doped tin oxide into powder, mixing the powder with polycarbonate and lubricant paraffin, wherein the components in parts by weight are 35 parts, 60 parts and 5 parts respectively, meanwhile, adding 3 parts of rhenium heptoxide serving as other auxiliary materials, 10 parts of an organic phosphorus flame retardant, 6 parts of tea polyphenol and 6 parts of rosin resin, uniformly mixing, adding into a double-screw extruder, heating at nine sections, extruding, cooling, drawing strips, air-drying and granulating to obtain the high-transmittance infrared blocking polycarbonate color master batch.
2. The method for preparing the polycarbonate color master batch with high infrared transmission barrier property according to the claim 1, wherein in the step 1), the stannous salt is one or the combination of stannous chloride or stannous sulfate; the strong acid is one or the combination of hydrochloric acid or sulfuric acid; the carbonate is one or the combination of sodium carbonate, potassium carbonate or lithium carbonate.
3. The method for preparing the high-transmittance infrared-blocking polycarbonate color master batch according to claim 1, wherein in the step 2), the indium salt is one or a combination of indium chloride or indium sulfate; the cesium salt is one or a combination of cesium chloride or cesium sulfate.
4. The preparation method of the polycarbonate color master batch with high infrared transmission and barrier properties of claim 1, wherein in the step 3), the cross section of the rod-shaped precursor is 3mm x 2.1mm, and the length of the rod-shaped precursor is 20 mm; the temperature programming rate is 10-15 ℃/min.
5. The preparation method of the high-transmittance infrared-blocking polycarbonate color master batch according to claim 1, wherein in the step 4), the nine-stage processing temperature of the twin-screw extruder is set as follows: the temperature in the first zone is 130 ℃, the temperature in the second zone is 185 ℃, the temperature in the third zone is 238 ℃, the temperature in the fourth zone is 250 ℃, the temperature in the fifth zone is 260 ℃, the temperature in the sixth zone is 260 ℃, the temperature in the seventh zone is 255 ℃, the temperature in the eighth zone is 230 ℃ and the temperature in the ninth zone is 180 ℃.
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CN107686602A (en) * | 2017-10-31 | 2018-02-13 | 上海稀美师塑料着色科技有限公司 | A kind of preparation method of infrared absorption Masterbatch |
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