CN114380344A - Preparation method of alumina modified soda-lime glass bead filter material - Google Patents
Preparation method of alumina modified soda-lime glass bead filter material Download PDFInfo
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- CN114380344A CN114380344A CN202011134704.XA CN202011134704A CN114380344A CN 114380344 A CN114380344 A CN 114380344A CN 202011134704 A CN202011134704 A CN 202011134704A CN 114380344 A CN114380344 A CN 114380344A
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- RHZUVFJBSILHOK-UHFFFAOYSA-N anthracen-1-ylmethanolate Chemical compound C1=CC=C2C=C3C(C[O-])=CC=CC3=CC2=C1 RHZUVFJBSILHOK-UHFFFAOYSA-N 0.000 description 1
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Images
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a preparation method of an alumina modified soda-lime glass bead filter material, which comprises the following steps: screening the obtained soda-lime glass microsphere raw material by a screen with a specific mesh number, sequentially and repeatedly cleaning the raw material by using deionized water, ethanol and acetone, and then carrying out acid washing by using a human-eating acid solution to remove organic impurities on the surface; adding an aluminum chloride solution and a sodium hydroxide solution, baking the mixture in an oven for 24 hours, and putting the baked mixture into a muffle furnace for high-temperature calcination to obtain the modified soda-lime-glass bead filter material attached with the alumina, wherein the modified soda-lime-glass bead filter material has better removal effect on negative electric pollutants such as micro-plastics and escherichia coli in water. The alumina modified soda-lime glass bead filter material obtained by the invention is more convenient in approach and cheaper in price, is more beneficial to removing micro-plastics in water, and can improve the treatment efficiency of the filter and the quality of the effluent.
Description
Technical Field
The invention belongs to the field of preparation of environment-friendly materials and treatment of drinking water, and particularly relates to a preparation method of an alumina modified soda-lime glass bead filter material.
Background
In the industrial process of water and drinking water purification and wastewater treatment, the quality of the filtration process often determines the treatment efficiency and effluent quality of a water plant. Filtration generally refers to a process flow in which impurities in water are trapped by a granular filter material layer such as quartz sand, thereby clarifying the water. The filtration can not only remove suspended matters in water so as to reduce turbidity, but also reduce BOD, COD, heavy metal ions and grease. In recent years, the water shortage condition is increasingly serious, the water quality standard is increasingly improved, and the traditional quartz sand filter material gradually exposes some inherent defects in the use process, such as negative surface charge, few surface gaps, small specific surface area, small porosity and the like. Secondly, the national requirements for energy conservation and emission reduction, the development of green cycle sustainable economy and the improvement of environmental governance are gradually improved, and the exploitation and processing of quartz sand filter materials belong to the high-pollution industry, so that the price of quartz sand is continuously increased in recent years. Therefore, the traditional quartz sand production and processing technology cannot meet the requirements of energy conservation and emission reduction at the present stage.
On the other hand, micro plastic is widely distributed in natural environment as a novel pollutant. Since the latest research was released from the society of us researchers in association with gastroenterology week in europe in 2018, 10, and 22 days after finding micro-plastics in bottled water, it was first confirmed that as many as 9 different kinds of micro-plastics were found in humans, and thus all societies around the world began to focus on the problem of micro-plastics, and a report named "micro-plastics in drinking water" was published by the world health organization in 2019. The traditional water treatment process can treat more than 70% of large-particle-size micro-plastics, and the filtering link plays an irreplaceable role. However, the zeta potential of the quartz sand filter material or other types of filter materials such as anthracite, ceramic and the like is negative, and the zeta potential of the micro plastic is also negative, so that the micro plastic with extremely small particle size is difficult to intercept in the filtering process due to the same electrical property. Besides micro-plastics, the zeta potential of most of other common pollutants such as bacteria, antibiotics, grease and the like is negative. According to the DLVO theory, when the zeta potential of the filter material is improved, the adsorption of pollutants in water in the filtering process is facilitated, and therefore the effluent quality is improved.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides a preparation method of an alumina modified soda-lime glass bead filter material aiming at the defects of negative surface charge, less surface gap, small specific surface area, small porosity and the current situation that the use cost is increased year by year in the traditional quartz sand filter material in the prior art.
The purpose of the invention is realized by the following technical scheme.
According to the preparation method of the alumina modified soda-lime glass bead filter material, after the soda-lime glass bead raw material is subjected to surface pretreatment and cleaning, alumina is attached to the surface, so that the charged functionalization of the soda-lime glass bead filter material is realized, and the modified soda-lime glass bead filter material with a specific mesh number is prepared.
The method specifically comprises the following steps:
(1) surface pretreatment of soda-lime glass beads
Screening a certain amount of soda-lime glass bead raw materials through a screen with a specific mesh number, and repeatedly cleaning the raw materials for 5-6 times by using high-grade pure absolute ethyl alcohol; sequentially putting the cleaned soda-lime glass microsphere raw materials into beakers filled with deionized water, ethanol and acetone, and performing ultrasonic treatment for 10min respectively; putting the glass bead raw material subjected to ultrasonic cleaning into a human-eating acid solution, and then carrying out water bath acid cleaning for 2 hours at the temperature of 95 ℃; repeatedly washing acid liquor remained on the glass beads with deionized water after water bath pickling is finished, and then putting the glass beads into absolute ethyl alcohol for storage for later use;
(2) modified treatment of soda-lime glass beads
Weighing the soda-lime glass beads pretreated in the step (1), and putting the soda-lime glass beads into an oven to be dried for later use; preparing sufficient aluminum chloride solution and sodium hydroxide solution, adding the aluminum chloride solution and the sodium hydroxide solution into the soda-lime glass beads, uniformly stirring, and putting the mixture into the oven again to be dried for 24 hours; in order to ensure that the filter material is heated uniformly, the filter material is stirred once every hour in the early stage of heating, and is taken out after being heated for 24 hours; repeating the above operation once; finally, adding an aluminum chloride solution and a sodium hydroxide solution into the filter material, and uniformly stirring; then, placing the mixture into a muffle furnace, drying for a certain time, and taking out; after the filter material is cooled, washing the filter material by tap water to remove coatings which are not firmly adhered to the surface; and (3) rinsing for three times by using distilled water, and drying for later use to obtain the alumina modified soda-lime glass bead filter material.
In the step (1), the particle size of the soda-lime glass beads is 20-40 meshes, the volume fraction of the absolute ethyl alcohol is 99.8%, the volume fraction of the acetone is 99.5%, the human eating acid solution is composed of concentrated sulfuric acid and hydrogen peroxide, and the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7: 3.
in the step (2), the concentration of the aluminum chloride solution is 3mol/L, the concentration of the sodium hydroxide solution is 10mol/L, and the dosage ratio of the aluminum chloride solution to the sodium hydroxide solution is 20: 1; and putting the pretreated soda-lime glass microspheres into a 50 ℃ oven for drying for later use, putting the soda-lime glass microspheres into the 100 ℃ to 120 ℃ oven for drying for 24 hours after adding an aluminum chloride solution and a sodium hydroxide solution and uniformly stirring, and setting the temperature of the muffle oven to be 240 ℃ to 550 ℃.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
the invention realizes the attachment of positive electric adsorption points on the surface and the accurate control of the grain diameter of the filter material. Compared with the traditional quartz sand filter material, the filter material is lower in price and less in surface pores and gullies, and due to the fact that positive electricity on the surface of the filter material adsorbs point positions, according to the DLVO theory, the filter material can effectively remove micro plastic and other negative electricity pollutants in water while keeping the original filtering performance, and has economic value and environmental protection significance.
Drawings
FIG. 1 is an SEM picture of modified soda-lime glass beads made of alumina in step two of example 1 of the present invention;
FIG. 2 is a diagram showing a modified alumina spectrum of soda-lime glass beads in step two of example 1;
FIG. 3 shows the zeta potential test results of the soda-lime glass beads modified with alumina in step two of example 1.
Detailed Description
The invention is further described below with reference to the figures and examples. This example is provided for a better understanding and is not intended to limit the invention in any way.
According to the preparation method of the alumina modified soda-lime glass bead filter material, disclosed by the invention, through a large amount of experimental researches, after the soda-lime glass bead raw material is subjected to surface pretreatment and cleaning, alumina is attached to the surface, so that the charged functionalization of the soda-lime glass bead filter material is realized, and the modified soda-lime glass bead filter material with a specific mesh number of alumina adsorption sites attached to the surface is successfully prepared. The method specifically comprises the following steps:
step one, performing surface pretreatment on the soda-lime glass beads
Screening a certain amount of soda-lime glass bead raw materials through a screen with a specific mesh number, and repeatedly cleaning the raw materials for 5-6 times by using absolute ethyl alcohol of superior grade pure (GR); sequentially putting the cleaned soda-lime glass microsphere raw materials into beakers filled with deionized water, ethanol and acetone, and performing ultrasonic treatment for 10min respectively; putting the glass bead raw material subjected to ultrasonic cleaning into a human-eating acid solution, and then carrying out water bath acid cleaning for 2 hours at the temperature of 95 ℃; and after the water bath pickling is finished, repeatedly washing the acid liquor remained on the glass beads with deionized water, and then putting the glass beads into absolute ethyl alcohol for storage for later use. The main purpose of this step is to clean the surface of the soda-lime glass beads of organic impurities.
The method is characterized in that cheap soda-lime glass beads purchased from manufacturers are used as raw materials, the particle size range is 20-40 meshes, the stacking volume is 200ml, homogeneous glass beads or inhomogeneous glass beads are used according to experimental requirements, and the pickled soda-lime glass bead raw materials are stored by adopting absolute ethyl alcohol, so that the influence of impurities in the air on the surface potential of the glass beads is isolated as far as possible. The volume fraction of the absolute ethyl alcohol is 99.8%, the volume fraction of the acetone is 99.5%, the human eating acid solution is composed of concentrated sulfuric acid and hydrogen peroxide, and the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7: 3.
step two, modifying the soda-lime glass beads
Weighing the soda-lime glass beads pretreated in the step one, and putting the soda-lime glass beads into a 50 ℃ oven for drying for later use; preparing enough aluminum chloride (AlCl)3) Adding the solution and a sodium hydroxide (NaOH) solution into the soda-lime glass beads, uniformly stirring, and putting into an oven at 100-120 ℃ again for baking for 24 hours; to ensure filteringUniformly heating, stirring once every one hour in the early stage of heating, and taking out the filter material after heating for 24 hours; repeating the above operation once; finally, aluminum chloride (AlCl) was added to the filter material3) Uniformly stirring the solution and a sodium hydroxide (NaOH) solution; then, putting the mixture into a muffle furnace, baking the mixture for a certain time (6 to 12 hours) at the temperature of between 240 and 550 ℃, and taking the mixture out; after the filter material is cooled, the filter material is slowly washed by tap water to remove coatings which are not firmly adhered to the surface; and (3) rinsing for three times by using distilled water, and drying for later use to obtain the alumina modified soda-lime glass bead filter material.
Wherein the concentration of the aluminum chloride solution is 3mol/L, the concentration of the sodium hydroxide solution is 10mol/L, and the dosage ratio of the aluminum chloride solution to the sodium hydroxide solution is 20:1, aiming at obtaining aluminum chloride (AlCl) when the amount of the sodium hydroxide (NaOH) solution is small3) The following chemical reaction with sodium hydroxide (NaOH) takes place: AlCl3+3NaOH＝3NaCl+Al(OH)3↓. Followed by 2Al (OH) in a high temperature environment3＝Al2O3+3H2And O, so that the adhesion of the alumina on the surface of the soda-lime glass microsphere is realized. When the sodium hydroxide (NaOH) solution is excessive, aluminum hydroxide precipitation cannot be normally generated, but AlCl occurs3+4NaOH＝3NaCl+NaAlO2The reaction of +2H2O is not favorable for the formation and adhesion of alumina in a high-temperature environment. The zeta potential of the alumina in the neutral water environment is a positive value, the zeta potential of the soda-lime glass beads in the neutral water environment is a negative value, and after the alumina is attached to the surfaces of the soda-lime glass beads, an adsorption potential of a positive potential is constructed on the surfaces of the glass beads of a negative potential, so that the adsorption effect on negative electric pollutants is improved.
After the alumina modified soda-lime glass bead filter material is prepared by the method, the characterization is carried out by using SEM and energy spectrum analysis, so as to verify whether the alumina is attached to the surface of the soda-lime glass bead, the zeta potential of the soda-lime glass bead filter material before and after modification is measured by using a CADzeta potential meter, and the change of the surface potential property of the filter material is observed.
(1) And measuring the surface components of the modified soda-lime glass beads by using SEM and energy spectrum analysis.
Taking the modified sodium-calcium glass obtained in the second stepSpraying gold on the glass bead filter material to prepare a sample, putting the sample into a tank, vacuumizing, adjusting voltage, contrast and brightness, searching a proper area by using a scanning electron microscope to take a picture, carrying out common energy spectrum scanning by using X rays, and analyzing and obtaining the concentration of various elements forming the sample material by using an X-ray energy spectrum analysis and detection method. Wherein the vacuum reaches 5 x 10-3Pa, the voltage is 20kv when the dot scanning is performed.
Scanning Electron Microscopy (SEM) uses secondary Electron signal imaging to observe the surface morphology of a sample, i.e. Scanning the sample with a very narrow Electron beam, and generating various effects by the interaction between the Electron beam and the sample, wherein the secondary electrons can generate an enlarged appearance on the surface of the sample. This image is built up chronologically as the sample is scanned, i.e. a point-by-point imaging method is used to obtain a magnified image. The most common method of electron microscopy is X-ray Energy Dispersive Spectroscopy (EDS). The method has component analysis function. Firstly, elements contained in a sample are identified through automatic qualitative analysis, and then the concentration of each element forming the sample material is obtained through semi-quantitative analysis and X-ray intensity.
(2) The Zeta potential of the filter material before and after modification was measured using a Zeta potential analyzer on the solid surface of zetaccad.
And (3) taking a proper amount of the soda-lime glass bead filter material sample pretreated in the first step, filling the sample into a zetacCAD sample filling column, introducing a sodium chloride electrolyte, adding a mixed phosphate solution, controlling the pH to be 7, and reading the zeta potential of the soda-lime glass bead filter material before modification.
Similarly, a proper amount of modified soda-lime glass bead filter material sample treated in the second step is taken and filled into a zetaccad sample filling column, a sodium chloride electrolyte is introduced, a mixed phosphate solution is added, the ph is controlled to be 7, and at the moment, the zeta potential of the modified soda-lime glass bead filter material is read.
Wherein the sample packed column has a diameter of 1.45cm and a length of 1.8cm, the sodium chloride electrolyte has a concentration of 0.019mol/L and a conductivity of 2.67mS/cm, and the mixed phosphate solution has a concentration of 0.025mol/L, resulting in an increase in conductivity to 3.4 mS/cm. The soda-lime glass beads before and after modification have no conductivity, and the conductivity of a sample needs to be enhanced through metal spraying sample preparation, so that the SEM shooting effect is improved.
The ZetacAD solid surface Zeta potential analyzer is a Zeta potential analyzer for directly measuring flowing potential/flowing current, and helps scientific human eyes to improve and adjust surface characteristics in the field of chemistry in material science. The method is suitable for large particles, fibers and flat surfaces deposited, or curved glue or hollow fiber samples penetrated by the electrolyte under a pressure gradient for scientific research, and is suitable for solid and powder materials with different shapes and sizes, such as polymers, textiles, ceramics, glass and the like.
Example 1:
the method comprises the following steps: sieving soda-lime glass beads with a stacking volume of 200ml by using a 30-32 mesh sieve, and repeatedly cleaning the raw materials for 5-6 times by using absolute ethyl alcohol with 99.8% of grade-superior purity (GR); sequentially putting the cleaned soda-lime glass microsphere raw materials into beakers filled with deionized water, ethanol and acetone, and performing ultrasonic treatment for 10min respectively; putting the glass bead raw material subjected to ultrasonic cleaning into a 'human-eating acid' solution (the volume ratio of concentrated sulfuric acid to hydrogen peroxide is 7: 3), and then carrying out water bath acid cleaning for 2 hours at the temperature of 95 ℃; and after the water bath pickling is finished, repeatedly washing the acid liquor remained on the glass beads with deionized water, and then putting the glass beads into absolute ethyl alcohol for storage for later use.
Step two: weighing 30g of pretreated soda-lime glass microspheres, and putting the microspheres into an oven (50 ℃) for drying for later use; preparing aluminium chloride (AlCl)3) Adding the solution of 3mol/L and the solution of 10mol/L of sodium hydroxide (NaOH) into the soda-lime glass beads, uniformly stirring, and putting the mixture into an oven (100 ℃) again to be dried for 24 hours; in order to ensure that the filter material is heated uniformly, the filter material is stirred once every one hour in the early stage of heating, and the filter material is taken out after being heated for 24 hours; repeating the above operation once; finally, a suitable amount of aluminum chloride (AlCl) is added to the filter material3) Uniformly stirring the solution and a sodium hydroxide (NaOH) solution with the dosage ratio of 20: 1; then, placing the mixture into a muffle furnace at 240 ℃, drying for 6 hours and taking out; after the filter material is cooled, the filter material is slowly washed by tap water to remove coatings which are not firmly adhered to the surface; washing with distilled water for three times, and oven drying to obtain aluminum oxideA sodium calcium glass bead filter material.
Step three: taking a proper amount of the sample treated in the second step, spraying gold to prepare a sample, putting the sample into a tank, and vacuumizing to 5 x 10-3Pa, adjusting the voltage to 20kv, contrast and brightness, using a scanning electron microscope to find a suitable area for photographing, as shown in FIG. 1, performing common energy spectrum scanning with X-rays, and analyzing and obtaining the concentrations of various elements constituting the sample material by adopting an X-ray energy spectrum analysis and detection method, as shown in FIG. 2.
Step four: and (3) taking a proper amount of the sample treated in the second step, directly filling the sample into a column with the diameter of 1.45cm and the length of about 1.8cm, and introducing a sodium chloride electrolyte, wherein the electrolyte is 0.13% of NaCl (0.019mol/L) in mass fraction and has the initial conductivity of 2.67 mS/cm. When the pH value is controlled to be 7, the mixed phosphate (0.025mol/L) is added to cause the conductivity to rise to 3.4mS/cm, and the zeta potential of the modified soda-lime glass bead filter material is read, as shown in FIG. 3.
Example 2:
the method comprises the following steps: sieving soda-lime glass beads with a sieve of 20-22 meshes and a stacking volume of 200ml, and repeatedly washing the raw materials for 5-6 times by using absolute ethyl alcohol with 99.8% of grade-superior purity (GR); sequentially putting the cleaned soda-lime glass microsphere raw materials into beakers filled with deionized water, ethanol and acetone, and performing ultrasonic treatment for 10min respectively; putting the glass bead raw material subjected to ultrasonic cleaning into a 'human-eating acid' solution (the volume ratio of concentrated sulfuric acid to hydrogen peroxide is 7: 3), and then carrying out water bath acid cleaning for 2 hours at the temperature of 95 ℃; and after the water bath pickling is finished, repeatedly washing the acid liquor remained on the glass beads with deionized water, and then putting the glass beads into absolute ethyl alcohol for storage for later use.
Step two: weighing 30g of pretreated soda-lime glass microspheres, and putting the microspheres into an oven (50 ℃) for drying for later use; preparing aluminium chloride (AlCl)3) Adding the solution of 3mol/L and the solution of 10mol/L of sodium hydroxide (NaOH) into the soda-lime glass beads, uniformly stirring, and putting the mixture into the oven (110 ℃) again to bake for 24 hours; in order to ensure that the filter material is heated uniformly, the filter material is stirred once every one hour in the early stage of heating, and the filter material is taken out after being heated for 24 hours; repeating the above operation once; finally, a suitable amount of aluminum chloride (AlCl) is added to the filter material3) The solution is dissolved in sodium hydroxide (NaOH)Uniformly stirring the solution with the dosage ratio of 20: 1; then, placing the mixture into a muffle furnace at 350 ℃, drying for 8 hours, and taking out; after the filter material is cooled, the filter material is slowly washed by tap water to remove coatings which are not firmly adhered to the surface; and (3) rinsing for three times by using distilled water, and drying for later use to obtain the alumina modified soda-lime glass bead filter material.
Step three: taking a proper amount of the sample treated in the second step, spraying gold to prepare a sample, putting the sample into a tank, and vacuumizing to 5 x 10-3Pa, adjusting the voltage to 20kv, contrast and brightness, using a scanning electron microscope to search for a suitable area for photographing, using X-rays to perform common energy spectrum scanning, and analyzing and obtaining the concentration of each element forming the sample material by adopting an X-ray energy spectrum analysis and detection method.
Step four: and (3) taking a proper amount of the sample treated in the second step, directly filling the sample into a column with the diameter of 1.45cm and the length of about 1.8cm, and introducing a sodium chloride electrolyte, wherein the electrolyte is 0.13% of NaCl (0.019mol/L) in mass fraction and has the initial conductivity of 2.67 mS/cm. When the pH value is controlled to be 7, the mixed phosphate (0.025mol/L) is added to cause the conductivity to rise to 3.4mS/cm, and the zeta potential of the modified soda-lime glass bead filter material is read.
Example 3:
the method comprises the following steps: sieving soda-lime glass beads with a sieve of 20-22 meshes and a stacking volume of 200ml, and repeatedly washing the raw materials for 5-6 times by using absolute ethyl alcohol with 99.8% of grade-superior purity (GR); sequentially putting the cleaned soda-lime glass microsphere raw materials into beakers filled with deionized water, ethanol and acetone, and performing ultrasonic treatment for 10min respectively; putting the glass bead raw material subjected to ultrasonic cleaning into a 'human-eating acid' solution (the volume ratio of concentrated sulfuric acid to hydrogen peroxide is 7: 3), and then carrying out water bath acid cleaning for 2 hours at the temperature of 95 ℃; and after the water bath pickling is finished, repeatedly washing the acid liquor remained on the glass beads with deionized water, and then putting the glass beads into absolute ethyl alcohol for storage for later use.
Step two: weighing 30g of pretreated soda-lime glass microspheres, and putting the microspheres into an oven (50 ℃) for drying for later use; preparing aluminium chloride (AlCl)3) Adding the solution of 3mol/L and the solution of 10mol/L of sodium hydroxide (NaOH) into the soda-lime glass beads, uniformly stirring, and putting the mixture into an oven (120 ℃) again to be dried for 24 hours; to ensure filteringUniformly heating, stirring once every one hour in the early stage of heating, and taking out the filter material after heating for 24 hours; repeating the above operation once; finally, a suitable amount of aluminum chloride (AlCl) is added to the filter material3) Uniformly stirring the solution and a sodium hydroxide (NaOH) solution with the dosage ratio of 20: 1; then, placing the mixture into a muffle furnace at 550 ℃, drying for 12 hours and taking out; after the filter material is cooled, the filter material is slowly washed by tap water to remove coatings which are not firmly adhered to the surface; and (3) rinsing for three times by using distilled water, and drying for later use to obtain the alumina modified soda-lime glass bead filter material.
Step three: taking a proper amount of the sample treated in the second step, spraying gold to prepare a sample, putting the sample into a tank, and vacuumizing to 5 x 10-3Pa, adjusting the voltage to 20kv, contrast and brightness, using a scanning electron microscope to search for a suitable area for photographing, using X-rays to perform common energy spectrum scanning, and analyzing and obtaining the concentration of each element forming the sample material by adopting an X-ray energy spectrum analysis and detection method.
Step four: and (3) taking a proper amount of the sample treated in the second step, directly filling the sample into a column with the diameter of 1.45cm and the length of about 1.8cm, and introducing a sodium chloride electrolyte, wherein the electrolyte is 0.13% of NaCl (0.019mol/L) in mass fraction and has the initial conductivity of 2.67 mS/cm. If the pH value needs to be controlled to be 7, the mixed phosphate (0.025mol/L) is added to cause the conductivity to rise to 3.4mS/cm, and the zeta potential of the soda-lime glass bead filter material before modification is read.
While the present invention has been described in terms of its functions and operations with reference to the accompanying drawings, it is to be understood that the invention is not limited to the precise functions and operations described above, and that the above-described embodiments are illustrative rather than restrictive, and that various changes and modifications may be effected therein by one skilled in the art without departing from the scope or spirit of the invention as defined by the appended claims.
Claims (4)
1. The preparation method of the alumina modified soda-lime glass bead filter material is characterized in that after the soda-lime glass bead raw material is subjected to surface pretreatment and cleaning, alumina is attached to the surface to realize the charged functionalization of the soda-lime glass bead filter material, so that the modified soda-lime glass bead filter material with a specific mesh number is prepared.
2. The preparation method of the alumina modified soda-lime glass bead filter material as claimed in claim 1, which is characterized by comprising the following steps:
(1) surface pretreatment of soda-lime glass beads
Screening a certain amount of soda-lime glass bead raw materials through a screen with a specific mesh number, and repeatedly cleaning the raw materials for 5-6 times by using high-grade pure absolute ethyl alcohol; sequentially putting the cleaned soda-lime glass microsphere raw materials into beakers filled with deionized water, ethanol and acetone, and performing ultrasonic treatment for 10min respectively; putting the glass bead raw material subjected to ultrasonic cleaning into a human-eating acid solution, and then carrying out water bath acid cleaning for 2 hours at the temperature of 95 ℃; repeatedly washing acid liquor remained on the glass beads with deionized water after water bath pickling is finished, and then putting the glass beads into absolute ethyl alcohol for storage for later use;
(2) modified treatment of soda-lime glass beads
Weighing the soda-lime glass beads pretreated in the step (1), and putting the soda-lime glass beads into an oven to be dried for later use; preparing sufficient aluminum chloride solution and sodium hydroxide solution, adding the aluminum chloride solution and the sodium hydroxide solution into the soda-lime glass beads, uniformly stirring, and putting the mixture into the oven again to be dried for 24 hours; in order to ensure that the filter material is heated uniformly, the filter material is stirred once every hour in the early stage of heating, and is taken out after being heated for 24 hours; repeating the above operation once; finally, adding an aluminum chloride solution and a sodium hydroxide solution into the filter material, and uniformly stirring; then, placing the mixture into a muffle furnace, drying for a certain time, and taking out; after the filter material is cooled, washing the filter material by tap water to remove coatings which are not firmly adhered to the surface; and (3) rinsing for three times by using distilled water, and drying for later use to obtain the alumina modified soda-lime glass bead filter material.
3. The preparation method of the alumina modified soda-lime glass bead filter material as claimed in claim 2, wherein in step (1), the particle size of the soda-lime glass beads is 20-40 meshes, the volume fraction of the absolute ethyl alcohol is 99.8%, the volume fraction of the acetone is 99.5%, the "edible acid" solution is composed of concentrated sulfuric acid and hydrogen peroxide, and the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7: 3.
4. the preparation method of the alumina modified soda-lime glass bead filter material as claimed in claim 2, wherein the concentration of the aluminum chloride solution in the step (2) is 3mol/L, the concentration of the sodium hydroxide solution is 10mol/L, and the ratio of the dosage of the aluminum chloride solution to the dosage of the sodium hydroxide solution is 20: 1; and putting the pretreated soda-lime glass microspheres into a 50 ℃ oven for drying for later use, putting the soda-lime glass microspheres into the 100 ℃ to 120 ℃ oven for drying for 24 hours after adding an aluminum chloride solution and a sodium hydroxide solution and uniformly stirring, and setting the temperature of the muffle oven to be 240 ℃ to 550 ℃.
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| CN115518459A (en) * | 2022-08-25 | 2022-12-27 | 上海凯工石油装备科技有限公司 | Production process of green glass filter material |
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