CN109052465B - Glass bead-nano titanium dioxide compound and preparation process thereof - Google Patents
Glass bead-nano titanium dioxide compound and preparation process thereof Download PDFInfo
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Abstract
The invention discloses a preparation process of a glass bead-nano titanium dioxide compound. The nano titanium dioxide is embedded into the surfaces of the glass beads at high temperature in a high-temperature adhesion mode, and when the glass beads are cooled, nano titanium dioxide particles can be firmly adhered to the surfaces of the glass beads. The method comprises the following specific steps: putting the glass beads pre-loaded with the nano titanium dioxide particles into a muffle furnace; setting the temperature of high-temperature calcination at 450-500 ℃; setting the high-temperature calcination time to be 1-3 h. The preparation process is simple, and the asphalt composition is applied to asphalt pavements and can effectively degrade automobile exhaust.
Description
Technical Field
The invention belongs to the field of road engineering, and particularly relates to a preparation process of a glass bead-nano titanium dioxide compound.
Background
The nano titanium dioxide is an environment-friendly material with no toxicity, high temperature resistance and good chemical stability, so the nano titanium dioxide is widely applied to industries such as pigments, cosmetics and the like. In addition, the nano titanium dioxide has excellent oxidation performance in the sun, so the material is widely applied to the fields of air purification, sewage treatment, medical disinfection and the like.
The application range of the nano titanium dioxide also depends on a loaded carrier, and the glass beads are a material with good light transmission performance and can provide sufficient illumination conditions for the nano titanium dioxide, so that the nano titanium dioxide can exert strong oxidation capacity. The glass beads are used as carriers, so that the application range of the nano titanium dioxide can be enlarged.
Disclosure of Invention
According to the invention, a High temperature adhesion mode is developed, nano titanium dioxide is embedded into the surface of glass beads at High temperature, and when the glass beads are cooled, nano titanium dioxide particles can be firmly adhered to the surface of the glass beads. The preparation process can apply the glass bead-nano titanium dioxide compound to the asphalt pavement, can degrade the automobile exhaust under the illumination condition, and has good social benefit and popularization and use value.
The invention relates to a preparation process of a glass bead-nano titanium dioxide compound, which comprises an experimental material of the preparation process of the glass bead-nano titanium dioxide compound, a preparation process of the glass bead-nano titanium dioxide compound and an analysis of a bonding process mechanism.
The glass bead-nano titanium dioxide composite comprises the following experimental materials:
glass micro-beads (Na)2O-B2O3-SiO2) Anatase Nano titanium dioxide (Nano-TiO)2) (ii) a Glass beads Na2O-B2O3-SiO2With anatase Nano-TiO2The mass ratio of 900-. The glass beads Na2O-B2O3-SiO2In Na2O、B2O3、SiO2The mass fraction is 10-15 percent respectively、3-5％、68-72％。
A preparation process of a glass bead-nano titanium dioxide composite comprises the following experimental steps:
(1) dissolving nano titanium dioxide particles in water, adjusting the rotating speed of the high-speed shearing machine to 400-600r/min, and stirring for 3-5 minutes to form a nano titanium dioxide aqueous solution;
adding glass beads, adjusting the rotating speed of the high-speed shearing machine to 800-1000r/min, stirring for 8-10 minutes, and filtering and drying after the high-speed shearing machine uniformly stirs to obtain a mixture;
(2) putting the glass beads pre-loaded with the nano titanium dioxide particles into a muffle furnace; heating to 450-500 ℃ at the speed of 8-10 ℃/min; and after the heat preservation and calcination are carried out for 1-2h, the glass microsphere-nano titanium dioxide composite can be prepared by naturally cooling to room temperature.
The glass beads are obtained by corroding with a calcium hydroxide saturated solution, and the specific steps are that the glass beads are soaked in Ca (OH)2Preserving the heat for 12-14h at 15-20 ℃ in the saturated solution, filtering, washing and drying to obtain the corroded glass microspheres.
A preparation process of a glass bead-nano titanium dioxide composite comprises the following calcination temperature and time selection and bonding process mechanism:
(1) calcination temperature
The chemical formula of the glass beads is Na2O-B2O3-SiO2The basic component is sodium oxide (Na)2O), boron trioxide (B)2O3) And silicon dioxide (SiO)2) Three substances. Since the melting points of the three components are different from each other and the three substances are connected by stable chemical bonds, the glass beads have no fixed melting point and no single crystal phase.
Of the three substances, SiO2Has a melting point of 1650 ℃ and Na2The melting point of O is 1132 deg.C, and B2O3Has a melting point of 445 ℃, i.e. the glass microspheres are B at a temperature of 445 DEG C2O3Is liquid and has been melted. This provides a way for loading nano titanium dioxide particles.
In addition, there are three types of nano titanium dioxide in nature, i.e., a titanium ore type, a brookite type, and a rutile type, and the melting point and the boiling point of brookite type and anatase type titanium dioxide do not exist in practice, and only rutile type titanium dioxide has the melting point and the boiling point. The invention selects anatase nano titanium dioxide, the crystal phase of which can change along with the rise of temperature, and the nano TiO treated by heat treatment at 500 DEG C2All are anatase phases; 600 ℃ heat treated nano TiO2The sample began to have rutile appeared; nano TiO heat treated at 700 deg.C2The anatase phase of the sample is nearly disappeared; nano TiO heat treated at 800 deg.C2The samples were all rutile.
In order to ensure that the crystal phase of the nano titanium dioxide is not transformed and ensure that the nano titanium dioxide can be adhered to the surface of the glass microsphere. Due to B2O3Has a melting point of 445 ℃, has melted into liquid at the temperature, and the nano titanium dioxide does not have crystalline phase transformation at the temperature. Therefore, the calcination temperature of the glass bead-nano titanium dioxide composite is selected to be 450-500 ℃.
(2) Calcination time
The time selection for calcining the glass bead-nano titanium dioxide composite is determined according to the time for converting the crystalline phase of the nano titanium dioxide. The high-temperature calcination experiment in a laboratory shows that the anatase nano titanium dioxide is calcined at 300 ℃ for 3h, at 500 ℃ for 1-2h and at 800 ℃ for 30min-1h at 450-. At this calcination temperature and calcination time, substantially no crystal phase transformation occurs. Therefore, the calcination temperature is selected to be 450-500 ℃ according to the calcination temperature of the glass bead-nano titanium dioxide composite, and the calcination time is determined to be 1-2h at the temperature.
(3) Mechanism of bonding process
In the glass microsphere in the state of being preloaded with the nano titanium dioxide, the nano titanium dioxide particles only enter the microstructure on the surface of the glass microsphere, and the microstructure comprises gaps with ravines, vertical and horizontal gaps and uneven micropores. And the nano titanium dioxide particles and the glass beads do not have any physical and chemical adsorption behaviors.
During the high-temperature calcination of the glass bead-nano titanium dioxide composite, B2O3Has a melting point of 445 ℃, and when the calcination temperature exceeds 445 ℃, B2O3Is melted and becomes liquid. At this time, the nano titanium dioxide particles are gradually embedded into the molten B under the action of gravity2O3When the temperature is cooled, the nano titanium dioxide particles are firmly adhered to the surfaces of the glass micro beads. The mechanism of the bonding process is shown in fig. 1, and the effect after high-temperature bonding is shown in fig. 2.
In the technical scheme of the invention, the calcium hydroxide solution corrodes the glass beads and self-assembles into a cellular surface microporous structure, and considering that the nano titanium dioxide only needs to be loaded on the surfaces of the glass beads, the glass beads have the particle size of 15-150 mu m, the average particle size of 75 mu m and the wall thickness of 1-2 mu m, while the anatase nano TiO nano particles provided by the invention2Has a particle diameter of (10 nm). The chemical component of the glass beads is Na2O-B2O3-SiO2This is a blend of 3 substances, without a fixed melting point and a separate crystalline phase, the idea of the invention being mainly to mix Ca (OH) at 20 ℃2Is easy to react with SiO2The product of the reaction is calcium silicate (CaSiO)3) The chemical reaction is shown as a formula (1).
Ca(OH)2+SiO2＝CaSiO3+H2O (1)
Known from the formula (1), Ca (OH)2With SiO2The chemical reaction takes place, the concentration of the calcium hydroxide solution is 0.16 percent, and the main component of the glass beads is sodium borosilicate (Na)2O-B2O3-SiO2) Having a molar mass of 180g.mol-1，
SiO2The molar mass is 60g.mol-1. Therefore, SiO is required as calculated by the formula (2)2Has a mass of 0.1296 g. By adopting the technical scheme, the thickness of 10-30nm can be corroded on the surface of the glass microsphere, the nano titanium dioxide can be loaded, and the coating effect of the nano titanium dioxide layer is ensured.
FIG. 3 is a process of etching a glass bead surface; fig. 4 shows the structure of glass beads and the texture of the surface after etching.
Drawings
Fig. 1 is a mechanism diagram of a bonding process of nano titanium dioxide particles and glass beads during high-temperature calcination.
FIG. 2 is a high-temperature adhesion effect diagram of nano titanium dioxide particles on the surface of glass beads.
FIG. 3 shows the etching process of the glass bead surface.
Fig. 4 shows the structure of glass beads and the texture of the surface after etching.
FIG. 5 is an electron microscope scan of glass beads before etching.
FIG. 6 is an electron microscope scan of glass beads after erosion.
FIG. 7 shows the adhesion effect of glass beads and nano-titania particles at different calcination temperatures
FIG. 8460 ℃ shows the adhesion effect of calcination for different times.
FIG. 9 gas reaction chamber.
FIG. 10 is a schematic diagram of an automotive exhaust degradation reaction.
Fig. 11 is a rut plate coated with glass microsphere and nano-titania composite.
FIG. 12 shows the tail gas degradation effect of the coated nano-titania-loaded pavement.
Detailed Description
Example 1
1. Corrosion of glass beads
100g of Ca (OH) was placed in a beaker2A saturated solution; soaking glass beads in Ca (OH)2Stirring evenly in the saturated solution at the rotating speed of 1000 r/min; preserving the heat of the whole beaker in a constant temperature water tank, and preserving the heat of the whole beaker in the constant temperature water tank for 12-14h at the temperature of 20 ℃; filtering and washing with 200 mesh screen (0.075mm), and oven drying at 105 deg.C; and observing the microporous structure of the surface layer of the glass bead by using a microscope scanner.
The calcium hydroxide solution corrodes the glass beads and self-assembles into a cellular surface microporous structure, and the chemical component of the glass beads is Na2O-B2O3-SiO2This is a blend of 3 substancesWithout a fixed melting point and a separate crystalline phase, mainly Ca (OH)2With SiO2The product of the reaction is calcium silicate (CaSiO)3) The chemical reaction is shown as a formula (1).
Ca(OH)2+SiO2＝CaSiO3+H2O (1)
Known from the formula (1), Ca (OH)2With SiO2Chemical reaction taking place, 1mol SiO2At least 1mol of Ca (OH) is required2The reaction can be completed. In Experimental step 2, the concentration of the calcium hydroxide solution was 0.16% at 20 ℃, and 100g of the saturated solution was taken, so that the mass of the calcium hydroxide solution was 0.16g, Ca (OH)2Has a molar mass of 74g.mol-1Of general formula (2)
In the formula: m-molar mass (g.mol)-1)，
m-mass of substance (g);
n-amount of substance (mol).
Calculated 100g of the saturated solution contained 0.00216mol Ca (OH)2According to formula (1), then the corresponding SiO2Amount of substance with Ca (OH)2The same applies to 0.00216 mol. The main component of the glass beads selected in the experiment is sodium borosilicate (Na)2O-B2O3-SiO2) Having a molar mass of 180g.mol-1，SiO2The molar mass is 60g.mol-1. Therefore, SiO is required as calculated by the formula (2)2Has a mass of 0.1296 g. FIG. 5 is an electron microscope scanning image of the glass beads before corrosion, and FIG. 6 is an electron microscope scanning image of the glass beads after corrosion.
2. Determining the optimum calcination temperature
The calcination temperature of the glass bead-nano titanium dioxide composite is controlled by B in the glass beads2O3And the time selection of calcination is determined according to the time for the nano titanium dioxide to be in the crystal phase transformation. Through high-temperature calcination in laboratoryExperiments show that the anatase nano titanium dioxide is calcined for 3h at 300 ℃, 1-2h at 450-800 ℃ and 30min-1h at 600-800 ℃. At this calcination temperature and calcination time, substantially no crystal phase transformation occurs. Therefore, the calcination temperature is selected to be 450-500 ℃ according to the calcination temperature of the glass bead-nano titanium dioxide composite, and the calcination time is determined to be 1-2h at the temperature.
In order to determine the optimal calcination temperature and time of the glass bead-nano titanium dioxide composite, the glass bead-nano titanium dioxide composite is calcined for 1h at intervals of 10 ℃ within the temperature range of 450-500 ℃, and the adhesion effect of the glass beads and the nano titanium dioxide particles at different calcination temperatures is observed. The adhesion effect at different temperatures is shown in fig. 7.
As can be seen from FIG. 7, the difference of the adhesion effect between the glass beads and the nano-titania particles at different calcination temperatures is small, and the nano-titania particles adhered to the surfaces of the glass beads are relatively uniform. At the temperature of 450-460 ℃, the surface of the glass microsphere has no fracture surface, and the shape is very complete. However, with the increase of temperature, the glass beads have pores with different degrees from 470 ℃, and when the temperature reaches above 490 ℃, the glass beads are broken in a large scale, so that the nano titanium dioxide particles are difficult to attach. Therefore, the optimum calcination temperature of the composite of glass microspheres and nano-titania particles is 460 ℃ from the viewpoint of the degree of breakage of the glass microspheres.
3. Determination of optimum calcination time
After the optimal calcination temperature of the composite of the glass beads and the nano titanium dioxide particles is determined, the optimal calcination time needs to be determined, and the calcination temperature of the composite is selected to be within the range of 450-500 ℃ and determined to be 1-2h by the indoor laboratory high-temperature calcination experiment. At 460 ℃, the initial calcination time is 1h, and 30min is the interval, and the effect of adhesion of the glass microspheres and the nano titanium dioxide particles at different calcination temperatures is observed. The adhesion effect at different calcination times is shown in fig. 8.
As can be seen from FIG. 8, the adhesion effect of the glass microspheres and the nano-titania particles is almost the same within 1-2h, the glass microspheres and the nano-titania particles can be uniformly adhered, and the conditions of cracks and holes are not generated. Therefore, the optimum calcination time was determined to be 1 hour in view of the production time and the resources to be charged.
Example 2
1. Design of gas reaction box and tail gas degradation system
In order to verify the effect of the composite of the glass beads and the nano titanium dioxide on the degradation of the automobile exhaust, a closed gas reaction box and a set of system for degrading the automobile exhaust are designed in an experiment, and are respectively shown in fig. 9 and fig. 10.
2. Preparing the composite of the glass beads and the nano titanium dioxide into aqueous solution
Before the experiment of degrading the automobile exhaust, the glass beads and the nano titanium dioxide compound are prepared into aqueous solution, and the aqueous solution is coated on the rut plate after being uniformly stirred, as shown in fig. 11.
Preparing the formula of the glass bead and nano titanium dioxide compound aqueous solution. According to literature investigations, preliminary protocols for aqueous solution coating are: the recommended dosage of the photocatalytic aqueous solution is 350-500g/m2In which the photocatalytic material (Nano-TiO)2) The dosage of the photocatalyst is 3% -5% of the photocatalytic aqueous solution. The area of the track plate is 0.09m2And obtaining the following through conversion: one track plate needs about 31.5-45g of photocatalytic aqueous solution, Nano-TiO2The dosage is about 0.945g-2.25 g. In the experiment, the ratio of the nano titanium dioxide to the glass beads in the high-temperature adhesion process is 1:10, so that the usage amount of the nano titanium dioxide-glass bead composite is 9.45-22.5 g. In addition, in consideration of the workability of stirring the nano titanium dioxide-glass beads and water, the ratio of the nano titanium dioxide-glass beads to the aqueous solution is recommended to be 1:10, the dosage of the corresponding photocatalytic aqueous solution is 94.5-225 g.
Photocatalytic material (Nano-TiO) to be used in this experiment2) The amount of the Nano-TiO Nano-composite material is 4 percent of the photocatalytic aqueous solution, and about 31.5 to 45g of the photocatalytic aqueous solution is needed for one track plate2The dosage is 1.606g, and the dosage of the nano titanium dioxide-glass bead compound is 17.67 g. According to the proportion of 1:10 of the nano titanium dioxide-glass beads to the aqueous solution, the dosage of the corresponding photocatalytic aqueous solution is 176.7 g.
3. Degradation of automobile exhaust
Uniformly coating the prepared photocatalytic aqueous solution on the surface of a rut plate, and drying the surface moisture in an oven at 40 ℃, wherein black cloth is required to be subjected to shading treatment in order to avoid light exposure in the whole process before formal experiments. The experimental process for degrading tail gas is as follows:
connection of devices
The experimental test piece used herein is a standard wheel-milled square rut test piece, the size is 30cm × 30cm × 5cm, and the actual reaction area is 30cm × 30 cm. And (4) putting the test piece block into a reaction box, and debugging a tail gas analyzer and connecting equipment. And introducing the tail gas into the gas reaction chamber for about 10min to remove air in the gas reaction chamber, closing the air outlet valve, introducing the tail gas for about 15min (the engine works at idle speed, and the rotating speed is 800r/min), and then closing the air inlet valve.
② data acquisition
Starting to collect the 1 st group of test data when the initial concentration of each harmful gas is stable as the initial tail gas concentration, and reading every 5min later, wherein the test objects mainly comprise HC, CO and CO2Gas concentration value of NOx. Because the tail gas analyzer has slow response to the concentration change of HC and NOx, the reading time is determined to be about 1min after the measurement is started, and the end time of each experimental test is determined to be 30min after the concentrations of HC and NOx are stable or return to zero.
(iii) evaluation of Tail gas degradation experiment
According to the technical route of the subject, the evaluation indexes of the automobile exhaust degradation experiment comprise the degradation rate, the single-stage degradation capability, the single-stage average degradation efficiency, the single-stage maximum degradation efficiency and the single-stage optimal reaction time period. Wherein, the time degradation rate is an index measured in real time, and the calculation of the rest evaluation indexes is shown as formulas (1) to (4).
Single stage degradation capacity:
in the formula: beta is single-stage degradability,%; c. CmaxIs the initial gas concentrationMaximum value, ml/m3；cminThe minimum value after the gas concentration is stabilized, ml.m-3。
Single stage average degradation rate:
in the formula:
ml.m for the single stage average degradation rate-3·min-1(ii) a And T is degradation reaction time min.
Single-stage maximum degradation efficiency:
in the formula: vmaxMaximum degradation efficiency in% for single stage; c. C1Is t1Gas concentration, ml · m, corresponding to time-3；c2Is t2Gas concentration, ml · m, corresponding to time-3；
Single-stage optimal reaction stage:
Top＝tf-ts (4)
in the formula: t isopMin for optimal reaction time; t is tfMin, the final moment when the degradation rate is higher than the average degradation rate; t is tsMin is the start of the degradation rate being higher than the average degradation rate.
Analysis of experimental results
At present, the self-designed gas reaction box and tail gas degradation system are adopted in the experiment, and the degradation effect of the loaded nano titanium dioxide pavement is preliminarily tried under the natural illumination condition. Test results show that the road surface loaded with the nano titanium dioxide has a good tail gas degradation effect, and the experimental results are shown in fig. 12. The evaluation indexes of the respective exhaust gas degradation experiments are shown in table 1.
TABLE 1 evaluation of NOx degradation in coated nano-titania-loaded pavement exhaust
| Type of load | Coated form |
| Light conditions | Natural illumination of light |
| Single stage degradation capability | 61.54％ |
| Single stage average degradation efficiency | 0.133mg/m3 |
| Maximum degradation efficiency in a single stage | 1.8mg/m3 |
| Single stage optimal reaction time period | 25-85min |
The tail gas degradation experiments show that the pavement loaded with the nano titanium dioxide has the most obvious effect of degrading nitrogen oxides in the tail gas of the automobile, the single-stage degradation capacity is 61.54%, and the single-stage average degradation efficiency is 0.133mg/m3The maximum degradation efficiency of the single stage is 1.8mg/m3The optimal reaction time period of the single stage is 25-85 min. In addition, as can be seen from fig. 12, the glass beads and the nano titanium dioxide composite also have a degradation effect on CO and on H2Degradation of S has little degradation effect. The experiments show that the composite of the glass beads and the nano titanium dioxide can degrade the automobile exhaust under the illumination conditionThe air purification has better effect.
Claims (2)
1. The preparation method of the glass bead-nano titanium dioxide compound is characterized in that the raw material comprises glass beads Na2O-B2O3-SiO2Anatase Nano-TiO titanium dioxide2(ii) a Glass beads Na2O-B2O3-SiO2With anatase Nano-TiO2The mass ratio of 900-:
dissolving nano titanium dioxide particles in water, adjusting the rotating speed of the high-speed shearing machine to 400-600r/min, and stirring for 3-5 minutes to form a nano titanium dioxide aqueous solution;
adding glass beads, adjusting the rotating speed of the high-speed shearing machine to 800-1000r/min, stirring for 8-10 minutes, filtering and drying after the high-speed shearing machine is uniformly stirred to obtain a mixture, placing the mixture in a muffle furnace, heating to 460 ℃ at the speed of 8-10 ℃/min, preserving heat, calcining for 1-2 hours, and naturally cooling to room temperature to obtain the glass bead-nano titanium dioxide compound; the glass beads are obtained by corroding with a calcium hydroxide solution, and the specific steps are that the glass beads are soaked in Ca (OH)2Preserving the heat for 12-14h at 15-20 ℃ in the saturated solution, filtering, washing and drying to obtain the corroded glass microspheres.
2. Use of the glass bead-nano titanium dioxide composite prepared according to claim 1 as an asphalt pavement material.
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