CN113880179A - Iron ion loaded composite PRB material of chitosan-coated quartz sand, preparation method and application thereof - Google Patents
Iron ion loaded composite PRB material of chitosan-coated quartz sand, preparation method and application 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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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
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- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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Abstract
The invention discloses a chitosan-coated quartz sand iron ion-loaded composite PRB material, a preparation method and application thereof, wherein quartz sand is used as a base material, chitosan is coated on the surface of the quartz sand, divalent iron ions are adsorbed on the surface of the coated quartz sand, a layer of irregular fold-shaped substance is formed on the surface of the chitosan-coated quartz sand iron ion-loaded composite PRB material, and a Fourier infrared spectrometer is used for scanning and analyzing the composite PRB material, so that an absorption peak superposed by stretching vibration peaks of-OH and N-H is formed at 3435cm-1, a C = C stretching vibration peak corresponding to 1625cm-1, and a deformation absorption peak of amino (-NH2) is formed at 1519 cm-1. According to the invention, chitosan is used as a basic organic matter, cheap and easily available quartz sand is selected as a support, and the organic mixture is coated on the quartz sand, so that the coating material taking the quartz sand as a base material is prepared, the dispersibility of the material is enhanced, the utilization efficiency is improved, the service life is prolonged, and the good effect of removing hexavalent chromium in underground water is realized.
Description
Technical Field
The invention belongs to the field of water treatment, and particularly relates to a chitosan-coated quartz sand loaded iron ion composite PRB material, a preparation method and application thereof.
Background
The underground water system is a basic component of an ecological system, rapid industrial development, urbanization expansion and agricultural production progress lead water resources to be threatened by heavy metal pesticide organic pollutants and the like, and have great responsibility for health and survival problems of human beings and other organisms. The degree of chromium pollution in the water body heavy metal pollution is second to lead pollution, and the chromium pollution mainly comes from daily production and life of people. The system of utilizing higher ground water in the industrial production process of chromium is a basic component of an ecosystem, and the rapid industrial development, the urbanization expansion and the progress of agricultural production cause water resources to be threatened by various organic pollutants of heavy metal pesticides and the like, thereby having great responsibility for the health and survival problems of human beings and other organisms. The degree of chromium pollution in the water body heavy metal pollution is second to lead pollution, and the chromium pollution mainly comes from daily production and life of people. The chromium is highly utilized in the industrial production process, for example, in the tanning industry, a large amount of chromium-containing synthetic tanning agent is used, but the utilization rate of the chromium is very low (60-70%), the residual chromium-containing waste liquid is discharged along with normal sewage, and the discharge of industrial waste water is one of important sources for causing chromium pollution.
Permeable Reactive Barrier (PRB) is an important remediation technology in groundwater pollution treatment. The PRB does not need to be additionally treated after being arranged in the underground water body, pollutants can be captured by the medium material in the PRB wall body along with the natural flow of the underground water body, when the pollutant removal capacity of the medium material reaches the upper limit or the conditions of deposition, blockage and the like exist, the medium material can be taken out from the PRB wall body for replacement and regeneration, or the PRB can be selected again according to the actual condition to construct the PRB, so that the unnecessary cost and other problems caused by the replacement of the material are avoided. Therefore, the PRB medium material must have high permeability, so that the polluted underground water can more easily pass through the reaction wall, and the natural water body is hardly disturbed, and the PRB medium material must be cheap and easily available due to the large using amount of the PRB medium material.
Disclosure of Invention
The invention aims to use quartz sand as a base material, coat chitosan with rich functional groups on the surface of the quartz sand, increase the types and the number of the utilized functional groups and increase the adsorption sites of the quartz sand so as to improve the adsorption effect of the quartz sand on hexavalent chromium, reduce the dosage of the chitosan and the cost, and obtain a reaction permeable wall material with low cost. In order to further increase the adsorption performance of the material, divalent iron ions are adsorbed on the surface of the coated quartz sand, and hexavalent chromium is removed by utilizing the reduction performance of the divalent iron ions.
In order to achieve the purpose, the invention adopts the technical scheme that:
a chitosan-coated quartz sand iron ion-loaded composite PRB material is prepared by taking quartz sand as a base material, coating chitosan on the surface of the quartz sand, adsorbing ferrous ions on the surface of the coated quartz sand, preparing a chitosan-coated quartz sand iron ion-loaded composite PRB material, forming a layer of irregular pleated substance on the surface of the chitosan-coated quartz sand iron ion-loaded composite PRB material, carrying out scanning analysis on the composite PRB material by using a Fourier infrared spectrometer, and carrying out scanning analysis on the composite PRB material, wherein an absorption peak superposed by a stretching vibration peak of-OH and an N-H at 3435cm < -1 >, a C = C stretching vibration peak corresponding to 1625cm < -1 >, and a deformation absorption peak of an amino group (-NH2) at 1519cm < -1 >.
The preparation method of the chitosan-coated quartz sand loaded iron ion composite PRB material comprises the following steps:
(1) at room temperature, 0.1-0.2g of glycan is weighed and added into 10mL of 2% acetic acid, and the mixture is stirred until the chitosan is completely dissolved into yellowish transparent solution;
(2) weighing 0.4g of quartz sand under the condition of continuous stirring, mixing the quartz sand into the completely dissolved solution (1), stirring the mixture for 60min, and adding 0.2mL of acrylic acid;
(3) then stirring for 60min, and adding 0.2mL of epoxy chloropropane into the solution (2);
(4) when the reaction time is 400min, under the stirring state, dropwise adding 1mL of 1% sodium tripolyphosphate solution into the solution (3), then dropwise adding 2mol/L NaOH solution, coagulating the mixed solution from paste to chitosan mixed micelle, and simultaneously clarifying and transparent the rest solution;
(5) standing and soaking the micelle in the solution (4) for 12h, washing residual NaOH solution with deionized water, filtering the mixture when the cleaning solution is neutral, drying, grinding and sieving with a 40-mesh sieve;
(6) and (3) taking 0.05g of the product in the step (5) to be placed in 50mL of 9g/L FeCl2 solution, oscillating for 400min in a constant-temperature shaking table at the rotating speed of 150r/min under the conditions of room temperature and no oxygen, washing for three times by using deionized water, and drying in vacuum to obtain the chitosan-coated quartz sand loaded iron ion composite PRB material.
The invention also provides a treatment method for treating hexavalent chromium polluted underground water, which comprises the following steps:
(1) adding the prepared chitosan-coated quartz sand-loaded iron ion composite PRB material into hexavalent chromium-polluted underground water, and uniformly mixing;
(2) and placing the mixed solution on a constant-temperature shaking table, wherein the rotating speed of the constant-temperature shaking table is 150r/min, and carrying out adsorption reaction.
Further: the concentration of hexavalent chromium ions in the hexavalent chromium polluted underground water is controlled to be 10-500 mg/L.
Preferably: the pH value of the hexavalent chromium polluted underground water is 3-8.
Further: the reaction temperature of the constant-temperature shaking table is 20-30 ℃.
Further: the dosage of the iron ion complex PRB material loaded on the chitosan-coated quartz sand is 1g/L-3 g/L.
Has the advantages that:
the chitosan has a large number of functional groups, but the types of the chitosan are few, and after the chitosan is grafted by using acrylic acid, the number and the types of the functional groups of the chitosan are enlarged, and the adsorption sites between the chitosan and Cr (VI) are increased. The acid resistance and stability of the uncrosslinked chitosan are slightly poor, and molecular chains of the chitosan are interwoven and wound after the chitosan is crosslinked by using epoxy chloropropane, so that the chemical stability of the chitosan is enhanced.
The quartz sand has a flat surface, a few pore structures, a low specific surface area and a low isoelectric point, and is most commonly used as a filter material to manufacture a filter bed in a water treatment process for intercepting fine particles, organic matters and the like in sewage. But the untreated quartz sand has limited effect on removing heavy metal pollution in the polluted water body. However, since the quartz sand has a stable structure, is low in price and wide in source, the invention selects the cheap and easily available quartz sand as a support, coats the organic mixture on the quartz sand, and prepares the coating material taking the quartz sand as a base material, thereby enhancing the dispersibility of the material, improving the utilization efficiency and prolonging the service life. The chitosan-coated quartz sand surface adsorbs Fe2+, so that Fe2+ directly participates in the reaction in an ion form, the affinity and the reducing force of the adsorbing material on hexavalent chromium can be increased, the good removing effect on hexavalent chromium is realized, and a reference way is provided for designing a PRB medium material for removing hexavalent chromium in underground water.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a scanning electron microscope picture of a chitosan-coated quartz sand loaded iron ion composite PRB material;
fig. 2 is a fourier infrared spectrum of the chitosan-coated quartz sand-loaded iron ion composite PRB material.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in 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.
Example 1
Preparation method of chitosan-coated quartz sand loaded iron ion composite PRB material
Weighing 0.2g of chitosan at room temperature, and adding the chitosan into 10mL of 2% acetic acid; stirring for 30min until chitosan is completely dissolved to form yellowish transparent solution;
weighing 0.4g of quartz sand under the condition of continuous stirring, mixing the quartz sand into the completely dissolved solution (1), stirring the mixture for 60min, and adding 0.2mL of acrylic acid;
then stirring for 60min, and adding 0.2mL of epoxy chloropropane into the solution (2);
when the reaction time is 400min, under the stirring state, dropwise adding 1mL of 1% sodium tripolyphosphate solution into the solution (3), then dropwise adding 2mol/L NaOH solution, coagulating the mixed solution into chitosan mixed micelle from paste, and simultaneously clarifying and transparent the rest solution;
and (3) statically soaking the micelle in the solution (4) for 12 hours, then washing residual NaOH solution by using deionized water, filtering the mixture when the cleaning solution is neutral, drying, grinding and sieving by using a 40-mesh sieve.
Introducing nitrogen, taking 0.05g of the product in the step (5) to 50mL of 9g/L FeCl2 solution, oscillating for 400min in a constant-temperature shaking table at the room temperature at the rotating speed of 150r/min, washing for three times by deionized water, and drying in a constant-temperature vacuum oven at the temperature of 60 ℃ to obtain the chitosan-coated quartz sand loaded iron ion composite PRB material.
The final product obtained in this way had the following characteristics:
referring to fig. 1, as shown in the figure, this is a scanning electron microscope picture of the composite PRB material, and a layer of irregular wrinkled substance is formed on the surface of the iron ion composite PRB material loaded on the chitosan-coated quartz sand, so that the specific surface area of the quartz sand is enlarged, and the absorption of hexavalent chromium ions is facilitated.
Referring to FIG. 2, scanning analysis of the PRB composite material by using a Fourier infrared spectrometer shows that the PRB composite material has an absorption peak superposed by stretching vibration peaks of-OH and N-H at 3435cm-1, a C = C stretching vibration peak corresponding to 1625cm-1 indicates that acrylic acid is successfully grafted on the PRB composite material, and a deformation absorption peak of amino (-NH2) at 1519cm-1 indicates that the surface of quartz sand is successfully coated with chitosan.
Example 2
The chitosan-coated quartz sand iron ion-loaded composite PRB material prepared in the embodiment 1 is applied to the treatment of simulating hexavalent chromium-polluted underground water, and comprises the following steps: 8 parts of 200mg/L chromium solution was prepared, and the pH of the reaction system was adjusted to 3, 4, 5, 6, 6.5, 7, 7.5 and 8 with 0.1mol/L HCl solution and 0.1mol/L NaOH solution, respectively. Adding the chitosan-coated quartz sand loaded iron ion composite PRB material, wherein the dosage of the adsorbent is 1 g/L. Respectively placing on a constant temperature shaking bed at 25 ℃. The rotation speed of the constant temperature shaking table is 150r/min, and the adsorption time is 300 min. After the reaction is finished, a syringe is used for sucking the supernatant, the adsorbent and the reaction solution are separated by using a standing and precipitating mode, and the adsorption process is finished. The content of hexavalent chromium which is not adsorbed in the reaction solution was measured by an ultraviolet spectrophotometry, and the result of the calculated adsorption amount is shown in table 1.
Table 1: influence of different pH values on removal of hexavalent chromium in underground water by chitosan-coated quartz sand loaded iron ion composite PRB material
| pH value | 3 | 4 | 5 | 6 | 6.5 | 7 | 7.5 | 8 |
| Adsorption Capacity (mg/g) | 97.9 | 86.0 | 82.5 | 68.8 | 53.3 | 43.1 | 25.4 | 16.6 |
As can be seen from Table 1, the adsorption effect was greatly affected by different pH values. The lower pH condition is favorable for removing hexavalent chromium ions, the pH value is increased, the adsorption capacity is gradually reduced, and the adsorption capacity reaches the optimal value of 97.9 mg/g when the pH value is 3.
Example 3
The chitosan-coated quartz sand iron ion-loaded composite PRB material prepared in the embodiment 1 is applied to the treatment of simulating hexavalent chromium-polluted underground water, and comprises the following steps: 3 parts of 200mg/L chromium solution was prepared, and the pH of the reaction system was adjusted to 3 with 0.1mol/L HCl solution. Adding the chitosan-coated quartz sand loaded iron ion composite PRB material, wherein the dosage of the adsorbent is 1 g/L. Placing on 20, 25 and 30 ℃ constant temperature shaking bed respectively. The rotation speed of the constant temperature shaking table is 150r/min, and the adsorption time is 300 min. After the reaction is finished, a syringe is used for sucking the supernatant, the adsorbent and the reaction solution are separated by using a standing and precipitating mode, and the adsorption process is finished. The content of hexavalent chromium which is not adsorbed in the reaction solution was measured by an ultraviolet spectrophotometry, and the calculated adsorption amount results are shown in table 2.
Table 2: influence of different temperatures on removal of hexavalent chromium in underground water by chitosan-coated quartz sand loaded iron ion composite PRB material
| Reaction temperature (. degree.C.) | 20 | 25 | 30 |
| Adsorption Capacity (mg/g) | 107.6 | 115.9 | 147.5 |
As can be seen from Table 2, the higher the reaction temperature is, the better the removal effect of the composite PRB material on hexavalent chromium is, and the adsorption capacity of the composite PRB material reaches 147.5 mg/g under the condition that the reaction temperature is 30 ℃.
Example 4
The chitosan-coated quartz sand iron ion-loaded composite PRB material prepared in the embodiment 1 is applied to the treatment of simulating hexavalent chromium-polluted underground water, and comprises the following steps: 200mg/L of chromium solution is prepared, and the pH value of the reaction system is adjusted to 3 by using 0.1mol/L of HCl solution. Adding the chitosan-coated quartz sand loaded iron ion composite PRB material, wherein the dosage of the adsorbent is 1 g/L. Respectively placing on a constant temperature shaking bed at 25 ℃. The rotation speed of the constant temperature shaking table is 150r/min, and the adsorption time is 10, 20, 30, 40, 50, 60, 120, 180, 240, 300, 360 and 480 min. After the reaction is finished, a syringe is used for sucking the supernatant, the adsorbent and the reaction solution are separated by using a standing and precipitating mode, and the adsorption process is finished. The content of hexavalent chromium which is not adsorbed in the reaction solution was measured by an ultraviolet spectrophotometry, and the calculated adsorption amount results are shown in table 2.
Table 3: influence of different reaction times on removal of hexavalent chromium in underground water by chitosan-coated quartz sand loaded iron ion composite PRB material
| Time (min) | 10 | 20 | 30 | 40 | 50 | 60 | 120 | 180 | 240 | 300 | 360 | 420 |
| Adsorption Capacity (mg/g) | 93.9 | 98.5 | 100.9 | 101.5 | 101.9 | 101.9 | 102.0 | 101.9 | 101.7 | 101.7 | 101.8 | 101.8 |
As can be seen from Table 3, as the reaction time increases, the adsorption amount of the composite PRB material to hexavalent chromium increases continuously, and the change of the adsorption effect is slight after 30min, so that the adsorption balance is basically achieved, and the adsorption amount of the composite PRB material to hexavalent chromium under the condition is 101.8 mg/g.
Example 5
The chitosan-coated quartz sand iron ion-loaded composite PRB material prepared in the embodiment 1 is applied to the treatment of simulating hexavalent chromium-polluted underground water, and comprises the following steps: eight chromium solutions with initial concentrations of 10, 20, 50, 100, 200, 300, 400 and 500mg/L are prepared, and the pH of the reaction system is adjusted to 3 by using 0.1mol/L HCl solution. Adding the chitosan-coated quartz sand loaded iron ion composite PRB material, wherein the dosage of the adsorbent is 1 g/L. Respectively placing on a constant temperature shaking bed at 25 ℃. The rotation speed of the constant temperature shaking table is 150r/min, and the adsorption time is 300 min. After the reaction is finished, a syringe is used for sucking the supernatant, the adsorbent and the reaction solution are separated by using a standing and precipitating mode, and the adsorption process is finished. The content of hexavalent chromium which is not adsorbed in the reaction solution was measured by an ultraviolet spectrophotometry, and the calculated adsorption amount results are shown in table 2.
Table 4: influence of different reaction concentrations on removal of hexavalent chromium in underground water by chitosan-coated quartz sand loaded iron ion composite PRB material
| Initial concentration (mg/L) | 10 | 20 | 50 | 100 | 200 | 300 | 400 | 500 |
| Adsorption Capacity (mg/g) | 7.7 | 20.4 | 42.5 | 81.6 | 114.2 | 126.0 | 153.1 | 182.7 |
As can be seen from Table 4, the increase in the initial concentration resulted in a concomitant increase in the adsorbed amount of the PRB composite material, and when the initial concentration was varied from 10 to 500mg/L, the adsorbed amount increased from 7.7 mg/g to 182.7 mg/g.
The chitosan has a large number of functional groups, but the types of the functional groups are few, and after the chitosan is subjected to grafting reaction by using acrylic acid, the number and the types of the functional groups of the chitosan can be enlarged, and the adsorption sites between the chitosan and hexavalent chromium are increased.
According to the invention, chitosan is used as a basic organic matter, cheap and easily available quartz sand is selected as a support, and the organic mixture is coated on the quartz sand to prepare the coating material taking the quartz sand as a base material, so that the dispersibility of the material is enhanced, the utilization efficiency is improved, the service life is prolonged, the good removing effect of hexavalent chromium is realized, and a reference way is provided for designing PRB (plant resource block) medium materials for removing hexavalent chromium in underground water.
The surface of the crosslinked chitosan adsorbs Fe2+, so that Fe2+ directly participates in the reaction in an ion form, and the affinity and the reduction capacity of the adsorbing material to hexavalent chromium can be improved.
Although embodiments of the present invention have been described above, it would be appreciated by those skilled in the art that changes may be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the claims.
Claims (8)
1. The utility model provides a compound PRB material of chitosan cladding quartz sand load iron ion which characterized in that: taking quartz sand as a base material, coating chitosan on the surface of the quartz sand, and adsorbing ferrous ions on the surface of the quartz sand coated with the chitosan to prepare a chitosan-coated quartz sand iron ion-loaded composite PRB material; a layer of irregular wrinkled substance is formed on the surface of the chitosan-coated quartz sand-loaded iron ion composite PRB material, scanning analysis is carried out on the composite PRB material by a Fourier infrared spectrometer, an absorption peak formed by overlapping a stretching vibration peak of-OH and an N-H vibration peak is formed at 3435cm < -1 >, a C = C stretching vibration peak corresponding to 1625cm < -1 >, and a deformation absorption peak of amino (-NH2) is formed at 1519cm < -1 >.
2. The preparation method of the chitosan-coated quartz sand-supported iron ion composite PRB material as claimed in claim 1, characterized by comprising the following steps:
(1) weighing 0.1-0.2g of chitosan at room temperature, adding the chitosan into 10mL of 2% acetic acid, and stirring until the chitosan is completely dissolved into yellowish transparent solution;
(2) weighing 0.4g of quartz sand under the condition of continuous stirring, mixing the quartz sand into the completely dissolved solution (1), stirring the mixture for 60min, and adding 0.2mL of acrylic acid;
(3) then stirring for 60min, and adding 0.2mL of epoxy chloropropane into the solution (2);
(4) when the reaction is carried out to 400mi, 1mL of 1% sodium tripolyphosphate solution is added into the solution (3) dropwise under the condition of keeping stirring, then 2mol/L NaOH solution is added dropwise, the mixed solution is coagulated into chitosan mixed micelle from paste, and meanwhile, the residual solution is clear and transparent;
(5) standing and soaking the micelle in the solution (4) for 12h, washing residual NaOH solution with deionized water, filtering the mixture when the cleaning solution is neutral, drying, grinding and sieving with a 40-mesh sieve;
(6) and (3) taking 0.05g of the product in the step (5) to be placed in 50mL of 9g/L FeCl2 solution, oscillating for 400min at the rotating speed of 150r/min in a constant-temperature shaking table under the conditions of room temperature and no oxygen, washing for three times by deionized water, and drying in vacuum to obtain the chitosan-coated quartz sand loaded iron ion composite PRB material.
3. The application of the chitosan-coated quartz sand-supported iron ion composite PRB material prepared by the method in claim 2 in water treatment.
4. The use according to claim 3, wherein said water is hexavalent chromium contaminated groundwater and the treatment method comprises the steps of:
(1) adding the chitosan-coated quartz sand-loaded iron ion composite PRB material prepared by the method in claim 2 into hexavalent chromium-polluted underground water, and uniformly mixing;
(2) placing the mixed solution on a constant-temperature shaking table, wherein the rotating speed of the constant-temperature shaking table is 150r/min, and carrying out adsorption reaction.
5. Use according to claim 3, characterized in that: the concentration of hexavalent chromium ions in the hexavalent chromium polluted underground water is controlled to be 10-500 mg/L.
6. The use according to claim 3, wherein the pH of said hexavalent chromium contaminated groundwater is from 3 to 8.
7. The use according to claim 3, wherein the reaction temperature of the constant temperature rocking bed is 20-30 ℃.
8. The use according to claim 3, wherein the chitosan-coated quartz sand-supported iron ion composite PRB material is used in an amount of 1g/L-3 g/L.
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| CN117884101A (en) * | 2024-01-15 | 2024-04-16 | 华中师范大学 | Chitosan modified zero-valent iron, preparation method thereof, zero-valent iron-based active sand filter filler and application |
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