CN110947362B - Ternary modified biochar for removing fluorine in water and preparation method thereof - Google Patents
Ternary modified biochar for removing fluorine in water and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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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
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
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- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to the technical field of wastewater treatment, and discloses ternary modified biochar for removing fluorine in water and a preparation method thereof, wherein biochar is added into a ternary modifier mixed solution containing lanthanum, iron and aluminum elements, and then base is slowly added to carry out enhanced modification on the biochar, so that the biochar surface forms an aluminum form, an iron form and a multi-metal layered double hydroxide colloid with high charge and high polymerization degree, and further the acid-base stability, the surface hydroxyl group, the anion exchange capacity and the isoelectric point of the modified biochar are improved, so that the fluorine removal performance of the modified biochar is improved, the application range of the modified biochar can be widened to be alkaline, and the pH application range of the modified biochar reaches 4-10. The fluorine removal rate can reach more than 90 percent when the fluorine is adsorbed.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to ternary modified biochar for removing fluorine in water and a preparation method thereof.
Background
Drinking water containing excessive fluoride for a long time may have adverse effects on human health. In the present-day fluorine removal technology field, adsorption is considered as a low-cost, simple and effective fluorine removal method. When the biochar is directly used as an adsorbing material, the defluorination effect is not ideal, and in the prior art, the biochar is modified by adopting metal so as to improve the adsorption capacity to fluorine.
In the design of the adsorption material, aiming at the characteristics of fluorine ions, the aspects of increasing the porosity and reducing the particle size, preferably mesoporous pores, large specific surface area, more positive charges, functional groups which have fluorine-like ion characteristics per se or doping elements and can perform anion exchange, such as hydroxyl, anions and the like, are usually considered. The aluminum (hydrogen) oxide has good fluorine-affinity characteristic and more positive charges, and can form a micropore, mesopore and macropore structure through process control, so that the aluminum-based adsorbent is selected as a main body and loaded on the biochar, which is a mainstream trend and an optimal selection. In recent years, rare earth elements Ce, La, Y and the like have been found to have excellent defluorination performance, but due to high cost, the rare earth elements are generally required to be compounded with other cheap metals such as aluminum for use, so that the good defluorination performance can be maintained, and the cost can be reduced. In the prior art, the lanthanum and aluminum salt mixed modification solution is used for modifying the biochar, the common modification method is a dipping-drying-sintering method, the fluorine removal efficiency of the obtained lanthanum and aluminum loaded modified biochar is still not ideal, and due to the low isoelectric point and the low anion exchange capacity, the pH application range of the material is in an acidic water body, the use is still limited, and the actual application requirements cannot be completely met.
Disclosure of Invention
The invention aims to provide a biochar adsorbing material for removing fluorine in water and a preparation method thereof.
In order to solve the technical problem, the invention provides a preparation method of ternary modified biochar for removing fluorine in water, which comprises the following steps:
1) dissolving lanthanum nitrate, ferric chloride and aluminum chloride in deionized water to prepare a ternary modifier mixed solution, and then adding biochar to stir to obtain a biochar-modifier-containing mixed stock solution;
2) dropwise adding a sodium hydroxide solution into the mixed stock solution containing the biochar-modifier obtained in the step 1) until the pH value is 7-8, and continuously stirring for 12 hours to obtain a modified product solution;
3) and (3) carrying out centrifugal separation on the modified product liquid obtained in the step 2), washing the precipitate obtained by the centrifugal separation, and drying to obtain the ternary modified biochar.
Preferably, the molar ratio of lanthanum nitrate to ferric chloride to aluminum chloride in step 1) is 1:2:3, and in the ternary modifier mixed solution, the concentration of lanthanum ions is 0.1-0.2 mol/L, the concentration of ferric ions is 0.2-0.4 mol/L, and the concentration of aluminum ions is 0.3-0.6 mol/L.
Preferably, the biochar in the step 1) is rice straw biochar.
Preferably, the mass-to-volume ratio of the biochar to the ternary modifier mixed solution in the step 1) is 1g:100 mL.
Preferably, the speed of dropwise adding the sodium hydroxide solution in the step 2) is 0.05-0.5 mL/min.
Preferably, the concentration of the sodium hydroxide solution in the step 2) is 2-4 mol/L.
Preferably, the washing in step 3) is specifically: the supernatant was washed with ultrapure water and was transparent.
Preferably, the drying temperature in the step 3) is 100-110 ℃.
The invention also provides the ternary modified biochar prepared by the preparation method.
Compared with the prior art, the method has the advantages that the biochar is added into the ternary modifier mixed solution containing lanthanum, iron and aluminum, and then the biochar is subjected to reinforced modification by slowly adding alkali, so that the surface of the biochar forms an aluminum form and an iron form with high charges and high polymerization degrees and a multi-metal layered double hydroxide colloid, the acid-base stability, the surface hydroxyl groups, the anion exchange capacity and the isoelectric point of the biochar are improved, the application range of the modified biochar can be widened to be alkaline besides the improvement of the fluorine performance, and the pH application range of the modified biochar reaches 4-10. The fluorine removal rate can reach more than 90 percent when the fluorine is adsorbed.
Detailed Description
For further illustration of the present invention, a detailed description of a biochar adsorbent material for removing fluorine from water and a method for preparing the same are provided below with reference to examples, but it should be understood that the descriptions are only for further illustration of the features and advantages of the present invention and are not intended to limit the claims of the present invention.
All of the starting materials of the present invention, without particular limitation as to their source, may be purchased commercially or prepared according to conventional methods well known to those skilled in the art.
Example 1
(1) And (3) carrying out high-temperature carbonization treatment on the rice straws to obtain the rice straw biochar.
(2) Dissolving 2.16g of lanthanum nitrate, 1.62g of ferric chloride and 2g of aluminum chloride in 100mL of deionized water to prepare a ternary modifier mixed solution, and then adding 1g of rice straw biochar to stir to obtain a biochar-modifier-containing mixed stock solution.
(3) And dropwise adding a sodium hydroxide solution with the concentration of 3mol/L into the obtained mixed stock solution containing the biochar-modifier at the speed of 0.2mL/min by using a peristaltic pump until the pH value is 7.5, and continuously stirring for 12h to obtain a modified product solution.
(4) And (3) carrying out centrifugal separation on the obtained modified product liquid, washing the precipitate obtained by the centrifugal separation, and drying at the temperature of 105 ℃ to obtain the ternary modified biochar made of rice straws.
(5) Performing a fluorine adsorption experiment on the obtained rice straw ternary modified biochar:
and (3) putting 40mL of aqueous solution containing 10mg/L of fluorine into a centrifugal tube, adjusting the pH to 8, adding 0.4g of the rice straw biochar adsorbing material obtained in the embodiment into the centrifugal tube, placing the centrifugal tube on a constant-temperature shaking table, shaking for 2 hours, centrifuging, measuring the residual concentration of fluorine in a supernatant by using an ion electrode method, and calculating the fluorine removal rate. The results are shown in Table 1.
Example 2
(1) And (3) carrying out high-temperature carbonization treatment on the rice straws to obtain the rice straw biochar.
(2) Dissolving 4.33g of lanthanum nitrate, 3.24g of ferric chloride and 4g of aluminum chloride in 100mL of deionized water to prepare a ternary modifier mixed solution, and then adding 1g of rice straw biochar to stir to obtain a biochar-modifier-containing mixed stock solution.
(3) And dropwise adding a sodium hydroxide solution with the concentration of 4mol/L into the obtained mixed stock solution containing the biochar-modifier at the speed of 0.05mL/min by using a peristaltic pump until the pH value is 7.5, and continuously stirring for 12h to obtain a modified product solution.
(4) And (3) carrying out centrifugal separation on the obtained modified product liquid, washing the precipitate obtained by the centrifugal separation, and drying at the temperature of 100 ℃ to obtain the ternary modified biochar made of rice straws.
(5) Performing a fluorine adsorption experiment on the obtained rice straw ternary modified biochar:
and (3) putting 40mL of aqueous solution containing 10mg/L of fluorine into a centrifugal tube, adjusting the pH to 4, adding 0.4g of the rice straw biochar adsorbing material obtained in the embodiment into the centrifugal tube, placing the centrifugal tube on a constant-temperature shaking table, shaking for 2 hours, centrifuging, measuring the residual concentration of fluorine in a supernatant by using an ion electrode method, and calculating the fluorine removal rate. The results are shown in Table 1.
Example 3
(1) And (3) carrying out high-temperature carbonization treatment on the rice straws to obtain the rice straw biochar.
(2) Dissolving 8.66g of lanthanum nitrate, 6.49g of ferric chloride and 8g of aluminum chloride in 100mL of deionized water to prepare a ternary modifier mixed solution, and then adding 1g of rice straw biochar to stir to obtain a biochar-modifier-containing mixed stock solution.
(3) And dropwise adding a sodium hydroxide solution with the concentration of 2mol/L into the obtained mixed stock solution containing the biochar-modifier at the speed of 0.5mL/min by using a peristaltic pump until the pH value is 7.5, and continuously stirring for 12h to obtain a modified product solution.
(4) And (3) carrying out centrifugal separation on the obtained modified product liquid, washing the precipitate obtained by the centrifugal separation, and drying at the temperature of 110 ℃ to obtain the ternary modified biochar made of rice straws.
(5) Performing a fluorine adsorption experiment on the obtained rice straw ternary modified biochar:
and (3) putting 40mL of aqueous solution containing 10mg/L of fluorine into a centrifugal tube, adjusting the pH to 10, adding 0.4g of the rice straw biochar adsorbing material obtained in the embodiment into the centrifugal tube, placing the centrifugal tube on a constant-temperature shaking table, shaking for 2 hours, centrifuging, measuring the residual concentration of fluorine in a supernatant by using an ion electrode method, and calculating the fluorine removal rate. The results are shown in Table 1.
Comparative example 1
(1) And (3) carrying out high-temperature carbonization treatment on the rice straws to obtain the rice straw biochar.
(2) Directly carrying out a fluorine adsorption experiment on the obtained rice straw biochar:
and (3) putting 40mL of aqueous solution containing 10mg/L of fluorine into a centrifugal tube, adjusting the pH to 4, adding 0.4g of the rice straw biochar adsorbing material obtained in the embodiment into the centrifugal tube, placing the centrifugal tube on a constant-temperature shaking table, shaking for 2 hours, centrifuging, measuring the residual concentration of fluorine in a supernatant by using an ion electrode method, and calculating the fluorine removal rate. The results are shown in Table 1.
Comparative example 2
(1) And (3) carrying out high-temperature carbonization treatment on the rice straws to obtain the rice straw biochar.
(2) And (3) taking 1g of the rice straw biochar, and fully stirring and soaking the rice straw biochar in 100mL of mixed solution containing 0.1mol/L lanthanum ion and 0.3mol/L aluminum ion for 12 hours to obtain modified product liquid.
(3) And (3) carrying out centrifugal separation on the obtained modified product liquid, washing the precipitate obtained by the centrifugal separation, and drying at the temperature of 110 ℃ to obtain the rice straw biochar adsorbing material.
(4) Directly carrying out a fluorine adsorption experiment on the obtained rice straw biochar:
and (3) putting 40mL of aqueous solution containing 10mg/L of fluorine into a centrifugal tube, adjusting the pH to 4, adding 0.4g of the rice straw biochar adsorbing material obtained in the embodiment into the centrifugal tube, placing the centrifugal tube on a constant-temperature shaking table, shaking for 2 hours, centrifuging, measuring the residual concentration of fluorine in a supernatant by using an ion electrode method, and calculating the fluorine removal rate. The results are shown in Table 1.
Comparative example 3
(1) And (3) carrying out high-temperature carbonization treatment on the rice straws to obtain the rice straw biochar.
(2) And (3) taking 1g of the rice straw biochar, and fully stirring and soaking the rice straw biochar in 100mL of mixed solution containing 0.1mol/L lanthanum ion and 0.3mol/L aluminum ion for 12 hours to obtain modified product liquid.
(3) And (3) carrying out centrifugal separation on the obtained modified product liquid, washing the precipitate obtained by the centrifugal separation, and drying at the temperature of 110 ℃ to obtain the rice straw biochar adsorbing material.
(4) Directly carrying out a fluorine adsorption experiment on the obtained rice straw biochar:
and (3) putting 40mL of aqueous solution containing 10mg/L of fluorine into a centrifugal tube, adjusting the pH to 10, adding 0.4g of the rice straw biochar adsorbing material obtained in the embodiment into the centrifugal tube, placing the centrifugal tube on a constant-temperature shaking table, shaking for 2 hours, centrifuging, measuring the residual concentration of fluorine in a supernatant by using an ion electrode method, and calculating the fluorine removal rate. The results are shown in Table 1.
TABLE 1 defluorination rate of rice straw biochar under different modification conditions
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Defluorination rate/%) | 96 | 92 | 91 | 15 | 78 | 41 |
As can be seen from Table 1, the rice straw biochar adsorbing material prepared by the preparation method disclosed by the invention is high in fluorine removal rate, and can still maintain a good fluorine removal rate in a wider acid-base range.
While there have been shown and described what are at present considered the fundamental principles and essential features of the invention and its advantages, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A preparation method of ternary modified biochar for removing fluorine in water is characterized by comprising the following steps:
1) dissolving lanthanum nitrate, ferric chloride and aluminum chloride in deionized water to prepare a ternary modifier mixed solution, and then adding biochar to stir to obtain a biochar-modifier-containing mixed stock solution; the biochar is rice straw biochar; the mass volume ratio of the biochar to the ternary modifier mixed solution is 1g:100 mL;
the molar ratio of lanthanum nitrate to ferric chloride to aluminum chloride is 1:2:3, and in the ternary modifier mixed solution, the concentration of lanthanum ions is 0.1-0.2 mol/L, the concentration of ferric ions is 0.2-0.4 mol/L, and the concentration of aluminum ions is 0.3-0.6 mol/L;
2) dropwise adding a sodium hydroxide solution into the mixed stock solution containing the biochar-modifier obtained in the step 1) until the pH value is 7-8, and continuously stirring for 12 hours to obtain a modified product solution;
3) and (3) carrying out centrifugal separation on the modified product liquid obtained in the step 2), washing the precipitate obtained by the centrifugal separation, and drying to obtain the ternary modified biochar.
2. The preparation method according to claim 1, wherein the dropping speed of the sodium hydroxide solution in the step 2) is 0.05 to 0.5 mL/min.
3. The preparation method according to claim 1, wherein the concentration of the sodium hydroxide solution in the step 2) is 2 to 4 mol/L.
4. The preparation method according to claim 1, wherein the washing in step 3) is specifically: the supernatant was washed with ultrapure water and was transparent.
5. The method according to claim 1, wherein the temperature of the drying in step 3) is 100 to 110 ℃.
6. The ternary modified biochar prepared by the preparation method according to any one of claims 1 to 5.
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| CN112121754A (en) * | 2020-09-27 | 2020-12-25 | 南通大学 | Composite adsorption material for removing fluorine in water and preparation method thereof |
| CN112121772A (en) * | 2020-09-27 | 2020-12-25 | 南通大学 | Defluorination wood film filtering device |
| CN112121773A (en) * | 2020-09-27 | 2020-12-25 | 南通大学 | Biological adsorption material for defluorination and preparation method thereof |
| CN113786806A (en) * | 2021-09-30 | 2021-12-14 | 南通大学 | Ternary modified sewage peat defluorinating agent and preparation method thereof |
| CN114405471B (en) * | 2022-01-27 | 2023-12-22 | 东南大学 | Aluminum-iron bimetal modified biochar dephosphorizing material and preparation method thereof |
| CN115259475B (en) * | 2022-08-23 | 2023-06-16 | 四川大学 | Method for removing fluorine by rare earth-assisted precipitation |
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