CN111252844B - Application of eggshell particles in bismuth-containing sewage treatment and use method thereof - Google Patents
Application of eggshell particles in bismuth-containing sewage treatment and use method thereof Download PDFInfo
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4881—Residues from shells, e.g. eggshells, mollusk shells
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The invention provides an application of eggshell particles in bismuth-containing sewage treatment and a using method thereof, wherein the eggshell particles are prepared by the following method: washing the eggshell with deionized water for 2-4 times, drying, air-drying at 30-50 ℃ for 9-11 h, and crushing to 0.4-0.5 mu m to obtain the eggshell particles. According to the invention, the eggshell particles are used as an adsorbent in the treatment of bismuth-containing sewage, and the alcoholic hydroxyl, methyl and carbonyl telescopic band functional groups on the eggshell surface interact with bismuth, so that the eggshell has the capacity of adsorbing bismuth, the bismuth content in the sewage can be effectively reduced, meanwhile, the eggshell has wide sources and low cost, and the application develops the new application of the eggshell and utilizes the eggshell waste to create new economic value.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to application of eggshell particles in bismuth-containing sewage treatment and a using method thereof.
Background
Contamination with many heavy metals is of concern, such as arsenic, bismuth, cadmium, chromium, cobalt, lead, manganese, mercury, nickel, platinum, silver, vanadium, and zinc. Bismuth is a rare and important component which is widely used in several fields, for example in the metallurgical and cosmetic industries as an additive substance for creams and hair dyes. In addition, it has well-defined properties in drug administration and can be used as an antibacterial agent against immunodeficiency infection in humans. However, bismuth has many adverse effects on the human body, such as kidney damage, halitosis, metallic taste and gingivitis, nausea, loss of appetite, weight loss, malaise, proteinuria, diarrhea, skin reactions, stomatitis, headache, fever, insomnia, depression, rheumatalgia, and high dose lethality. According to the world health organization, the allowable limit value of the concentration of bismuth in the natural water is 0.028 mg/L. The bismuth is released into the water body, so that the water body cannot be normally used. Therefore, it is necessary to clean and prevent bismuth before it enters the natural environment.
There are several conventional physical and chemical wastewater treatment techniques for removing contaminants from contaminated water. Of all the techniques, adsorption is the most popular technique because of its convenience, ease of handling and versatility. Natural or plant waste adsorbents are widely used in water treatment to replace the current expensive method of removing heavy metals from contaminated water. The activated carbon, the activated alumina and the ion exchange resin have strong removal capability to toxic heavy metals. However, these materials have certain drawbacks, and there is a need to find and develop a low cost, widely available, and large quantity of waste materials as a substitute. The eggshells are produced by several tons every day, most of the eggshells are sent to a refuse landfill, the eggshells cannot be effectively utilized, and the management cost is high. It is economically feasible to create new value using eggshell waste.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an application and a use method of eggshell particles in bismuth-containing sewage treatment, the eggshell particles are used as an adsorbent in the bismuth-containing sewage treatment, and alcoholic hydroxyl, methyl and carbonyl telescopic band functional groups on the surface of an eggshell interact with bismuth, so that the eggshell has the capacity of adsorbing bismuth, the bismuth content in the sewage can be effectively reduced, meanwhile, the eggshell has wide sources and low cost, and the application develops new application of the eggshell and creates new economic value by utilizing eggshell waste.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows: provides an application of eggshell particles in the treatment of bismuth-containing sewage.
Furthermore, the adding proportion of the eggshell particles in the bismuth-containing sewage is 3.125-50 g/L.
Furthermore, the adding proportion of the eggshell particles in the bismuth-containing sewage is 6.25 g/L.
Further, the eggshell particles are prepared by the following method: washing the eggshell with deionized water for 2-4 times, drying, air-drying at 30-50 ℃ for 9-11 h, and crushing to 0.4-0.5 mu m to obtain the eggshell particles.
Further, the eggshell is an eggshell of poultry or birds.
Furthermore, the eggshell is a chicken eggshell.
An adsorbent for bismuth-containing sewage comprises the eggshell particles.
The application method of the eggshell particles in the bismuth-containing sewage comprises the following steps: adding the eggshell particles into bismuth-containing sewage with the temperature of 40-50 ℃ and the pH value of 8 +/-0.5, and then stirring for 30-60 min to complete the treatment of the bismuth-containing sewage.
Further, the stirring speed is 140 to 160 rpm.
In summary, the invention has the following advantages:
1. according to the invention, the eggshell particles are used as an adsorbent in the treatment of bismuth-containing sewage, and a specific using method is provided, and the alcoholic hydroxyl, methyl and carbonyl telescopic band functional groups on the eggshell surface interact with bismuth, so that the eggshell has the capacity of adsorbing bismuth, the bismuth content in the sewage can be effectively reduced, meanwhile, the eggshell has wide sources and low development cost, and the application develops a new application of the eggshell, creates a new economic value by using eggshell waste, and also reduces the management cost.
2. The adsorption effect of the eggshell on bismuth is related to the reaction time, the addition amount of the eggshell, the temperature of sewage and the pH value. The adsorption amount of the eggshell to bismuth is increased along with the prolonging of the reaction time, the balance is achieved at 45min, and the removal rate reaches 94.10%. The initial rapid removal is due to the fact that a large number of effective binding sites exist on the surface of the eggshell, bismuth ions are easily adsorbed, and therefore the bismuth ions are rapidly removed. The large surface area of the adsorbent means that the number of available adsorption sites is sufficient in the initial stage, and as the reaction proceeds, these adsorption sites are availableSaturation progresses, and thus the adsorption rate decreases. The pH of the solution affects the functional groups on the egg shell that bind to the metal ions and the competition of the metal ions for the adsorbent surface active sites. The removal rate of the eggshell to the bismuth depends on the pH value, and when the pH value is 8, OH is added-React with bismuth ions to form a precipitate of double hydroxide. At a pH of less than 6, H+Competition with bismuth ions inhibits bismuth ions from binding to active sites on the adsorbent surface. The maximum removal rate obtained at pH 8 was 93.70%.
3. The removal rate of bismuth increases as the amount of eggshell gradually increases from 3.125g/L to 50 g/L. The removal rate is related to the amount of eggshell, since more adsorption sites are available at higher amounts; this trend is mainly due to the increase in the surface area of the eggshells and the increase in the adsorption activity. At a dose of 6.25g/L, the maximum removal rate of bismuth is 92.40%; further increasing the adsorbent amount (6.25-50 g/mL) has no significant effect on the adsorption rate of bismuth. The removal rate of bismuth ions is increased in the process that the temperature is increased between 40 and 50 ℃; the removal rate at 40 ℃ is 90.45 percent; the decrease in removal rate at 20 ℃ is due to the low temperature, since the molecules tend to move more and more from the adsorbent surface to the liquid phase, the boundary layer thickness tends to decrease, and hence the adsorption capacity decreases. One reason for the adsorption is that additional reactions initiated by the thermal cracking process form alkyne or alkene functional groups on the surface of the egg shell.
4. The eggshell has large specific surface area and high porous structure, thus having stronger adsorption capacity. Similarly, many tiny particles appear in the cavities on the surface of the eggshell, indicating that the eggshell may adsorb bismuth from the solution. In addition, the negative charge binding sites on the surface of the eggshell provide the eggshell with the ability to adsorb bismuth ions in aqueous solutions. From SEM images of the eggshells before and after adsorption, bismuth ions appear on the surfaces of the eggshells after adsorption. The image shows that there is a combination of small and large particles on the surface of the eggshell, similar to the uneven rough porous surface of the bronchiolar structure. EDS peaks show that bismuth does not exist in eggshells before adsorption, and the content of the bismuth in the eggshells after adsorption reaches 3.07%.
5. The actual interaction between the eggshell and bismuth exists, and the adsorption of the adsorbent material to the metal is realized byReactive groups and chemical bonds present on the material. From the FTIR spectrum, from 3435 to 3403cm-1The movement of (2) is stretching of-OH groups, and the difference between before and after adsorption is not large. Characteristic peaks were found between the eggshell surfaces, but at 2140.32cm-1After adsorption, a-C.ident.C bond appears. This bond refers to the alkyne or alkene bond formed by the reaction that occurs during thermal cracking. Adsorbing bismuth on the surface of eggshell, and then adsorbing bismuth on 3435, 2978, 2876, 2518, 1418, 774, 515 and 425cm-1The peaks at (A) are shifted to 3403, 2936, 2515, 1409, 791, 588 and 468cm respectively-1Here, it is illustrated that carboxyl groups, phenolic hydroxyl groups, aromatic rings, amino groups and aliphatic hydrocarbons are involved in the adsorption process.
Drawings
FIG. 1 shows the removal rate of bismuth ions by eggshells at different reaction times;
FIG. 2 shows the removal rate of bismuth by reacting eggshells at different pH values for 45 min;
FIG. 3 shows the removal rate of bismuth in eggshells at different pH values within 0-45 min;
FIG. 4 shows the bismuth removal rate of 45min reaction under different eggshell usage;
FIG. 5 shows the bismuth removal rate for different eggshell dosages within 0-45 min;
FIG. 6 shows the removal rate of bismuth ions in eggshells at different temperatures for 45 min;
FIG. 7 shows the removal rate of bismuth ions by eggshells at different reaction temperatures within 0-45 min;
fig. 8 is an SEM image of the eggshells before adsorption (1);
fig. 9 is an SEM image of the eggshells before adsorption (2);
FIG. 10 is an EDS spectrum of eggshells prior to adsorption;
fig. 11 is an SEM image of the eggshells after adsorption (1);
fig. 12 is an SEM image of the eggshells after adsorption (2);
fig. 13 is an SEM image of the eggshells after adsorption (3);
fig. 14 is an SEM image of the eggshells after adsorption (4);
figure 15 is an EDS spectrum of the eggshells after adsorption;
FIG. 16 is an FTIR spectrum of functional groups in eggshells before and after adsorption;
fig. 17 is an FTIR spectrum of functional group interactions in eggshells before and after adsorption.
Detailed Description
Example 1
The preparation method of the eggshell particles comprises the following steps: washing eggshell with deionized water for 3 times, drying, air drying at 40 deg.C for 10 hr, and pulverizing to 0.45 μm to obtain eggshell granule.
Example 2
Bismuth nitrite is adopted to prepare bismuth ion standard stock solution. A standard stock solution of bismuth ions was prepared by adding 1mL of nitric acid (65 vt%) to 1.4g of bismuth, followed by dilution to 1000mg/L with deionized water. The pH of the solution during the experiment was adjusted with 0.1M hydrochloric acid and 0.1M sodium hydroxide. The chemical reagents used in this study were purchased from Shanghai Aladdin Biotechnology Ltd.
0.25g of the eggshell particles obtained in example 1 was weighed and added to 40mL of bismuth ion standard stock solution (50mg/L) at 40 ℃ and pH 8, and then stirred at 150rpm while measuring the bismuth concentration in the solution at different reaction times, and the removal rate was calculated, the results of which are shown in FIG. 1.
As can be seen from FIG. 1, the adsorption amount of bismuth by the eggshell increases with the increase of the reaction time, and reaches equilibrium at 45min, and the removal rate reaches 94.10%. The initial rapid removal is due to the fact that a large number of effective binding sites exist on the surface of the eggshell, bismuth ions are easily adsorbed, and therefore the bismuth ions are rapidly removed. Since the surface area of the adsorbent is large, meaning that the number of available adsorption sites is sufficient in the initial stage, these adsorption sites gradually saturate as the reaction proceeds, and thus the adsorption rate decreases.
Example 3
0.25g of the eggshell particles obtained in example 1 was weighed, added to 40mL of bismuth ion standard stock solutions (50mg/L) having pH values of 2, 4, 6, 8, 10 and 12 at 40 ℃, and then stirred at 150rpm for 45min while measuring the bismuth concentration in the solution and calculating the removal rate, the results of which are shown in fig. 2 to 3.
As shown in FIGS. 2 to 3, the pH of the solution affects the functional groups on the eggshell that bind to the metal ions and the goldBelongs to the competition of ions on the surface active sites of the adsorbent. The removal rate of the eggshell to the bismuth depends on the pH value, and when the pH value is 8, OH is added-React with bismuth ions to form a precipitate of double hydroxide. At a pH of less than 6, H+Competition with bismuth ions inhibits bismuth ions from binding to active sites on the adsorbent surface. The maximum removal rate obtained at pH 8 was 93.70%.
Example 4
0.125g, 0.25g, 0.5g, 1g and 2g of the eggshell particles obtained in example 1 were weighed, respectively, added to 40mL of a bismuth ion standard stock solution (50mg/L) having a pH of 8 at 40 ℃, and then stirred at 150rpm for 45min, while the bismuth concentration in the solution was measured, and the removal rate was calculated, the results of which are shown in FIGS. 4 to 5.
As can be seen from FIGS. 4-5, the removal rate of bismuth increased as the amount of eggshell was gradually increased from 3.125g/L to 50 g/L. The removal rate is related to the amount of eggshell, since more adsorption sites are available at higher amounts; this trend is mainly due to the increase in the surface area of the eggshells and the increase in the adsorption activity. At a dose of 6.25g/L, the maximum removal rate of bismuth is 92.40%; further increasing the adsorbent amount (6.25-50 g/mL) has no significant effect on the adsorption rate of bismuth.
Example 5
0.25g of eggshell particles obtained in example 1 was weighed, added to 40mL of bismuth ion standard stock solution (50mg/L) having pH 8 at different temperatures of 20 ℃, 30 ℃, 40 ℃ and 50 ℃, and then stirred at 150rpm for 45min, while the bismuth concentration in the solution was measured, and the removal rate was calculated, the results of which are shown in fig. 6 to 7.
As can be seen from FIGS. 6 to 7, the removal rate of bismuth ions increases in the process of increasing the temperature between 40 ℃ and 50 ℃; the removal rate at 40 ℃ is 90.45 percent; the decrease in removal rate at 20 ℃ is due to the low temperature, since the molecules tend to move more and more from the adsorbent surface to the liquid phase, the boundary layer thickness tends to decrease, and hence the adsorption capacity decreases. One reason for the adsorption is that additional reactions initiated by the thermal cracking process form alkyne or alkene functional groups on the surface of the egg shell.
Example 6
SEM images and EDS spectra of the original eggshell before adsorption in example 1 and the eggshell after adsorption in example 2 at 45min are respectively obtained, wherein the SEM images of the original eggshell are shown in figures 8-9, the EDS spectra are shown in figure 10, the SEM images of the eggshell after adsorption are shown in figures 11-14, and the EDS spectra are shown in figure 15; and table 1 was prepared.
TABLE 1 EDS Spectrum of Eggshells
From the above, the eggshell has a large specific surface area and a highly porous structure, and thus has a strong adsorption capacity. Similarly, many tiny particles appear in the cavities on the surface of the eggshell, indicating that the eggshell may adsorb bismuth from the solution. In addition, the negative charge binding sites on the surface of the eggshell provide the eggshell with the ability to adsorb bismuth ions in aqueous solutions. From SEM images of the eggshells before adsorption (figures 8-9) and after adsorption (figures 11-14), bismuth ions appear on the surfaces of the eggshells after adsorption. The image shows that there is a combination of small and large particles on the surface of the eggshell, similar to the uneven rough porous surface of the bronchiolar structure. EDS peaks show that bismuth does not exist in eggshells before adsorption, and the content of the bismuth in the eggshells after adsorption reaches 3.07%. In fact, ground eggshell consists of 98.00% of calcium inorganic compounds (calcium carbonate, small amounts of magnesium carbonate, phosphoric acid) and 2% of other organic substances (proteins). These compounds interact with bismuth in the egg shell, forming the EDS spectrum peak.
From the SEM and EDS results, it can be seen that there is a real interaction between the eggshell and bismuth. The adsorption of the adsorbent material to the metal is due to active groups and chemical bonds existing on the material, and the infrared spectrum of the adsorbent material is shown in FIGS. 16-17. From 3435 to 3403cm-1The movement of (2) is stretching of-OH groups, and the difference between before and after adsorption is not large. Characteristic peaks were found between the eggshell surfaces, but at 2140.32cm-1After adsorption, a-C.ident.C bond appears. This bond refers to the alkyne or alkene bond formed by the reaction that occurs during thermal cracking. Adsorbing bismuth on the surface of eggshell, and then adsorbing bismuth on 3435, 2978, 2876, 2518, 1418, 774, 515 and 425cm-1The peak at the position is respectively shifted to 3403, 2936,2515. 1409, 791, 588 and 468cm-1Here, it is illustrated that carboxyl groups, phenolic hydroxyl groups, aromatic rings, amino groups and aliphatic hydrocarbons are involved in the adsorption process.
While the present invention has been described in detail with reference to the illustrated embodiments, it should not be construed as limited to the scope of the present patent. Various modifications and changes may be made by those skilled in the art without inventive step within the scope of the appended claims.
Claims (5)
1. The use method of the eggshell particles in the bismuth-containing sewage is characterized by comprising the following steps: adding the eggshell particles into bismuth-containing sewage with the temperature of 40-50 ℃ and the pH value of 8 +/-0.5, and then stirring for 30-60 min at the stirring speed of 140-160 rpm to finish the treatment of the bismuth-containing sewage;
the eggshell particles are prepared by the following method: washing the eggshell with deionized water for 2-4 times, drying, air-drying at 30-50 ℃ for 9-11 h, and crushing to 0.4-0.5 mu m to obtain the eggshell particles.
2. The method for using the eggshell particles in bismuth-containing wastewater as claimed in claim 1, wherein the proportion of the eggshell particles added in bismuth-containing wastewater is 3.125-50 g/L.
3. The method of using eggshell particles as recited in claim 1, wherein said eggshell particles are added to said bismuth-containing wastewater at a ratio of 6.25 g/L.
4. Method for using eggshell particles as in bismuth-containing wastewater according to claim 1, wherein said eggshells are avian or avian eggshells.
5. The method of using eggshell particles as recited in claim 1, wherein said eggshells are eggshells.
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