CN115121228B - Lanthanum modified carbon nanotube hydrogel as well as preparation method and application thereof - Google Patents
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Abstract
The invention provides a lanthanum modified carbon nano tube hydrogel and a preparation method and application thereof. According to the invention, ammonia water is selected as a pH regulator and a coprecipitation agent to prepare the lanthanum-modified carbon nanotube, and then the lanthanum-modified carbon nanotube is further prepared into hydrogel, so that the prepared lanthanum-modified carbon nanotube hydrogel adsorption material can have a better removal effect on phosphorus in sewage within a wider pH range (pH=3-10).
Description
Technical Field
The invention relates to the technical field of sewage treatment, in particular to lanthanum modified carbon nano tube hydrogel and a preparation method and application thereof.
Background
Eutrophication of water refers to the fact that nutrient substances such as nitrogen, phosphorus and the like are discharged into the water body due to human activities, so that algae in the water body are greatly propagated, the content of dissolved oxygen in the water body is greatly reduced, and the water body is odorized and a large number of aquatic organisms die. Phosphorus is one of the factors mainly causing eutrophication of water, and main pollution sources include domestic sewage and industrial wastewater, rainfall, snowfall, surface runoff, livestock manure in the breeding industry and the like. With the rapid development of economy, people overuse phosphate-containing fertilizers, so that excessive phosphorus in soil enters surface water, and the phosphorus content of the surface water is increased sharply. Excessive accumulation of phosphorus in the water body can lead algae to propagate in a large amount in the water, the content of dissolved oxygen in the water is rapidly reduced, fish and shrimp die due to hypoxia, the water quality is further deteriorated, and nausea-causing malodor is emitted. Algae in water increases, some of which contain algae toxins, which have an effect on the safety of people in drinking water.
At present, methods for removing phosphorus in water body include biological method, chemical method, membrane separation method, crystallization method, adsorption method and the like. The adsorption method is widely applied and researched due to the advantages of large capacity, low energy consumption, high speed, low pollution and the like. The existing adsorbent for removing phosphorus in water body mainly comprises biochar, hydrotalcite, metal oxide, waste residue, clay ore, other materials and modified substances thereof. The traditional adsorbent has poor special adsorption capacity for phosphate, the effect is not ideal, the modified adsorbent can well make up the defects of the traditional adsorbent, and the phosphate adsorption capacity is improved to a greater extent.
Lanthanum has stronger affinity for phosphate radical, and the specific surface area of the adsorption material modified by lanthanum is larger, which is favorable for the adsorption material to fully utilize the self void characteristic to physically intercept phosphorus element. The raw materials of the lanthanum-modified material generally adopt materials with larger porosity, such as natural clay materials, carbon-based materials, inorganic metal oxide materials and the like. The carbon nanotube is a one-dimensional nanoscale material, has the advantages of rich pore structure and larger specific surface area, and has the defects that the carbon nanotube is easy to generate agglomeration phenomenon in water, the adsorption capacity of the carbon nanotube is influenced, and modification is needed to reduce the agglomeration degree of the carbon nanotube, so lanthanum is considered to be introduced to modify the carbon nanotube. Meanwhile, the size of the powdery carbon nanotubes is too small, and there is a problem that solid-liquid separation and recycling are difficult after adsorbing contaminants.
Therefore, a phosphorus adsorption material which is cheap and easy to obtain, has excellent adsorption performance, is favorable for recycling and is ecological and environment-friendly needs to be designed and prepared.
Disclosure of Invention
Based on the defects that the existing water body phosphorus adsorption material is poor in adsorption capacity, harmful to ecology and difficult to separate phosphorus from the water body and then recycle the phosphorus, the invention aims to provide the preparation method of the lanthanum modified carbon nano tube hydrogel which is good in phosphorus adsorption effect and easy to separate and recycle from the water body.
Another object of the present invention is to provide a lanthanum-modified carbon nanotube hydrogel prepared by the preparation method.
The invention further aims to provide an application of the lanthanum modified carbon nano tube hydrogel in wastewater dephosphorization.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a preparation method of lanthanum modified carbon nano tube hydrogel comprises the following steps:
s1, fully and uniformly mixing carboxylated carbon nanotubes and soluble lanthanum salt in water to obtain a mixed solution, then adding ammonia water to adjust the pH value to 10.5-11, stirring to perform coprecipitation reaction, separating out a solid product, and freeze-drying to obtain lanthanum modified carbon nanotube powder;
s2, uniformly dissolving the lanthanum-modified carbon nanotube powder obtained in the step S1 and sodium alginate in water to obtain a hydrogel precursor mixed solution, and dripping the mixed solution into an aqueous solution of a cross-linking agent to obtain the lanthanum-modified carbon nanotube hydrogel.
According to the invention, the hydrogel is used as a carrier to optimize the separation effect of the phosphorus adsorption material and the water body, the hydrogel is used as a polymer material with a three-dimensional network structure, the original structure and performance of the polymer material can be maintained while the polymer material is remarkably swelled in water, the solid-liquid separation is facilitated, and the hydrogel can also play a certain role in protecting the lanthanum modified carbon nano tube, so that the polymer material has a higher phosphorus adsorption effect in a wider pH range. According to the invention, further research shows that in the preparation process of the lanthanum modified carbon nano tube, ammonia water is selected as a pH regulator and a coprecipitation agent, ammonium ions in the ammonia water are adsorbed to the surface of the carbon nano tube, so that the prepared hydrogel has a better and richer pore structure, the adsorption and storage of phosphorus are facilitated, and the ammonium ions can adsorb more phosphorus elements in a water body through the action of electrostatic adsorption, so that the prepared adsorbent lanthanum modified carbon nano tube hydrogel has a good phosphorus adsorption effect.
Preferably, the soluble lanthanum salt is at least one of lanthanum nitrate or lanthanum chloride.
Preferably, the carbon nanotubes in the carboxylated carbon nanotubes are at least one of single-walled carbon nanotubes or multi-walled carbon nanotubes.
Preferably, the mass ratio of the carboxylated carbon nanotubes to the soluble lanthanum salt is 1: (2-5).
Preferably, in the step S1, in the mixed solution formed by carboxylated carbon nanotubes and soluble lanthanum salt, the concentration of the carbon nanotubes is 1-5wt%, and too high concentration easily causes uneven dispersion of the carbon nanotubes, and the dispersion time length and the time cost are increased.
In step S1, the carbon nanotubes and the soluble lanthanum salt may be dispersed by a conventional (dispersing) mixing method, including but not limited to stirring, shaking or ultrasonic, preferably ultrasonic, method.
Preferably, the mixing in the step S1 is carried out at normal temperature (20-30 ℃), and the mixing time is 4-5 hours.
Conventional commercial ammonia may be used in the present invention.
Preferably, the stirring temperature of the coprecipitation reaction in the step S1 is 55-65 ℃ and the stirring time is 20-24 h. The coprecipitation is carried out at the temperature, so that lanthanum hydroxide precipitate can be uniformly loaded on the surface of the carbon nano tube.
Conventional solid-liquid separation means, including but not limited to at least one of centrifugation or suction filtration, may be used in step s1 to separate the solid product.
The solid product separated in the step S1 can be washed with water according to the need to remove residual ions.
Preferably, in the step S1, the freeze drying temperature is-20 to-40 ℃ and the vacuum degree is 13 to 40Pa.
Preferably, in the step s2, the mass ratio of the lanthanum-modified carbon nanotube powder to sodium alginate is (0.3-0.5): 1.
preferably, in the step S2, the concentration of sodium alginate in the hydrogel precursor mixed solution is 1-5 wt%.
Preferably, in the step s2, the cross-linking agent is at least one of lanthanum chloride or calcium chloride.
In step S2, after the hydrogel precursor mixed solution is dripped into the aqueous solution of the cross-linking agent, as the molecular structure of Sodium Alginate (SA) contains a large number of carboxyl and hydroxyl, the sodium alginate has stronger affinity, and under mild conditions, the hydrogel with an egg-box structure can be formed by crosslinking with divalent or multivalent cations through ionic bonds, so that the hydrogel precursor mixed solution liquid drops are converted from the solution to the gel, and the spherical lanthanum modified carbon nanotube hydrogel is formed.
Preferably, the concentration of the crosslinking agent in its aqueous solution is 1 to 5wt%.
The invention also protects the lanthanum modified carbon nano tube hydrogel prepared by the preparation method.
The application of the lanthanum modified carbon nano tube hydrogel in the wastewater dephosphorization is also within the protection scope of the invention.
Preferably, the lanthanum modified carbon nanotube hydrogel of the invention is used in sewage according to the weight ratio: phosphorus content in water= (10-125): 1.
compared with the prior art, the invention has the beneficial effects that:
according to the invention, ammonia water is selected as a pH regulator and a coprecipitation agent to prepare the lanthanum-modified carbon nanotube, and then the lanthanum-modified carbon nanotube is further prepared into hydrogel, so that the prepared lanthanum-modified carbon nanotube hydrogel adsorption material can have a better removal effect on phosphorus in sewage within a wider pH range (pH=3-10).
Drawings
Fig. 1 is an SEM image of the lanthanum modified carbon nanotube hydrogel prepared in example 1, wherein a is a spherical lanthanum modified carbon nanotube hydrogel particle, and b is a partial enlarged view;
FIG. 2 is a graph showing the relationship between the amount of lanthanum-modified carbon nanotube hydrogel prepared in example 1 and the amount of phosphorus removed and adsorbed;
FIG. 3 is a graph showing the adsorption performance of the lanthanum-modified carbon nanotube hydrogel prepared in example 1 in water with different phosphorus concentrations;
FIG. 4 is a graph showing the adsorption performance of the lanthanum modified carbon nanotube hydrogel prepared in example 1 in water under different pH conditions.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples and the accompanying drawings, but the examples are not intended to limit the present invention in any way. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art. The reagents and materials used in the present invention are commercially available unless otherwise specified.
Example 1
The embodiment provides a lanthanum-modified carbon nanotube hydrogel, and the preparation method thereof comprises the following steps:
s1, preparing lanthanum modified carbon nano tube powder
Adding 1g of carboxylated multiwall carbon nanotube into 100mL of water, carrying out ultrasonic treatment for 1h to obtain a uniformly dispersed carbon nanotube aqueous solution, then adding 3g of lanthanum chloride hexahydrate into the carbon nanotube aqueous solution, magnetically stirring for 4h at room temperature (20-30 ℃) to obtain a mixed solution, adding ammonia water into the mixed solution until the pH value is 11, heating to 60 ℃, stirring at constant temperature for 24h, centrifuging (3000 r/min) to obtain a solid material, washing the solid material with clear water (pouring the solid into a beaker, adding ultrapure water to a 500mL scale, magnetically stirring for 10min at 25 ℃, standing for 10-15 min, pouring out supernatant), and then carrying out freeze drying for 48h at-30 ℃ under the vacuum degree of 20Pa to obtain lanthanum modified carbon nanotube powder;
s2, preparing lanthanum modified carbon nano tube hydrogel
Adding 0.4g of the lanthanum-modified carbon nanotube powder prepared in the step S1 into 100mL of water, performing ultrasonic treatment for 1.5h, adding 1g of sodium alginate powder, and magnetically stirring at 60 ℃ for 5h to obtain a hydrogel precursor mixed solution;
weighing 12g of lanthanum chloride hexahydrate, adding the lanthanum chloride hexahydrate into 400mL of water, stirring until the lanthanum chloride hexahydrate is completely dissolved for use, sucking the mixed solution of the hydrogel precursor into a 20mL needle tube, and then dropwise adding the mixed solution into the lanthanum chloride solution to obtain the lanthanum modified carbon nanotube hydrogel.
Example 2
The present embodiment provides a lanthanum-modified carbon nanotube hydrogel, which is different from embodiment 1 in the preparation method thereof: lanthanum chloride hexahydrate was replaced with lanthanum nitrate hexahydrate.
Example 3
The present embodiment provides a lanthanum-modified carbon nanotube hydrogel, which is different from embodiment 1 in the preparation method thereof: in step S1, the pH is adjusted to 10.5.
Comparative example 1
This comparative example provides a lanthanum modified carbon nanotube hydrogel, which is prepared by a method different from that of example 1 in that: the ammonia water was replaced with sodium hydroxide.
Comparative example 2
The comparative example provides a lanthanum-modified carbon nanotube powder, which is obtained according to the method of step s1 in the example.
Performance testing
The properties of the lanthanum-modified carbon nanotube hydrogels obtained in the above examples and comparative examples were characterized, and specific test items, test methods and results are as follows:
1. morphology characterization: characterization is performed by using a Scanning Electron Microscope (SEM), the test results are shown in fig. 1, it can be seen from fig. 1 that the lanthanum-modified carbon nanotube hydrogel prepared in example 1 of the present invention has a loose surface lamellar structure, and granular protrusions can be observed, and the protrusions are embedded lanthanum-modified carbon nanotubes, which means that the lanthanum-modified carbon nanotube hydrogel has a plurality of adsorption sites for adsorbing phosphate, so that the adsorption capacity can be improved, and the results of other examples are similar to those of example 1.
2. Characterization of phosphorus adsorption performance in water:
1) Determination of the addition:
the mass ratio of the modified carbon nano tube hydrogel to the total phosphorus content of the water body containing phosphorus pollutants is 10/1-125/1 (namely, 0.1-1.25 g/L is added), the phosphate concentration in the water is 10mg/L, the adsorbent and the phosphorus solution are added into a conical flask for mixing and vibrating, the vibrating frequency is 160r/min, and the vibrating time is 14h. As a result, when the addition amount of the lanthanum-modified carbon nanotube hydrogel was increased from 0.1g/L to 1.25g/L, the removal rate was increased from 18.13% to 98.95% (FIG. 2), but the adsorption amount was decreased from 17.25mg/g to 7.53mg/g, and the addition amount of the adsorbent was considered to be 0.75g/L, considering the adsorption amount, the removal rate, and the cost control as a whole, as appropriate.
2) Adsorption performance at different phosphorus concentrations:
preparing an initial phosphorus solution by using potassium dihydrogen phosphate, preparing initial phosphorus concentrations of 5mgP/L, 10mgP/L and 20mgP/L respectively, and carrying out experiments, wherein the lanthanum-modified carbon nanotube hydrogel prepared by the above examples and comparative examples is used as an adsorbent, and the mass ratio of the lanthanum-modified carbon nanotube hydrogel to the total phosphorus content of the water body containing phosphorus pollutants is 75:1, carrying out experiments by adopting a plurality of conical flasks with 100mL, wherein the main method is to put the conical flasks filled with the phosphorus solution and the adsorbent into a constant temperature oscillator for oscillation, take out the conical flasks according to different time intervals to measure the residual phosphorus concentration in the conical flasks until the adsorption equilibrium is reached, calculate the equilibrium time and the phosphorus removal rate, and the results are shown in FIG. 3 and Table 1 in detail;
3) Adsorption properties at different pH:
the initial phosphorus concentration is 10mg/L, the pH values of phosphorus solutions in different conical flasks are respectively adjusted to be 2-12 by using HCl and NaOH, then the adsorbent is put into the conical flasks for mixing and shaking, the shaking frequency is 160r/min, the shaking time is 14h, and the adsorption test results are shown in table 1 of FIG. 4.
Table 1 results of adsorption performance test of adsorbents obtained in examples and comparative examples
From the above results, it can be seen that:
the lanthanum modified carbon nano tube hydrogel prepared by the invention is suitable for sewage with wider pH value, and has quicker balance time compared with a comparative example.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (9)
1. The preparation method of the lanthanum modified carbon nano tube hydrogel is characterized by comprising the following steps of:
s1, fully and uniformly mixing carboxylated carbon nanotubes and soluble lanthanum salt in water to obtain a mixed solution, then adding ammonia water to adjust the pH value to 10.5-11, stirring to perform coprecipitation reaction, separating out a solid product, and freeze-drying to obtain lanthanum modified carbon nanotube powder; the mass ratio of the carboxylated carbon nano tube to the soluble lanthanum salt is 1: (2-5);
s2, uniformly dissolving the lanthanum-modified carbon nanotube powder obtained in the step S1 and sodium alginate in water to obtain a hydrogel precursor mixed solution, and dripping the hydrogel precursor mixed solution into an aqueous solution of a cross-linking agent to obtain the lanthanum-modified carbon nanotube hydrogel.
2. The method of claim 1, wherein the soluble lanthanum salt is at least one of lanthanum nitrate or lanthanum chloride.
3. The method for preparing a lanthanum modified carbon nanotube hydrogel according to claim 1, wherein the temperature of the mixing in step s1 is 20 to 30 ℃.
4. The method for preparing lanthanum-modified carbon nanotube hydrogel according to claim 1, wherein the temperature of the coprecipitation reaction in step s1 is 55-65 ℃ for 20-24 hours.
5. The method for preparing lanthanum-modified carbon nanotube hydrogel according to claim 1, wherein in step s2, the mass ratio of lanthanum-modified carbon nanotube powder to sodium alginate is (0.3-0.5): 1.
6. the method of claim 1, wherein the cross-linking agent in step s2 is at least one of lanthanum chloride or calcium chloride.
7. The method for preparing a lanthanum modified carbon nanotube hydrogel according to claim 1, wherein the dissolution temperature in step s2 is 40-50 ℃.
8. A lanthanum-modified carbon nanotube hydrogel, which is prepared by the method for preparing the lanthanum-modified carbon nanotube hydrogel according to any one of claims 1 to 7.
9. The use of the lanthanum-modified carbon nanotube hydrogel of claim 8 in wastewater dephosphorization.
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