CN113750972B - Chromium ion adsorbent and preparation method thereof - Google Patents
Chromium ion adsorbent and preparation method thereof Download PDFInfo
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- CN113750972B CN113750972B CN202111243766.9A CN202111243766A CN113750972B CN 113750972 B CN113750972 B CN 113750972B CN 202111243766 A CN202111243766 A CN 202111243766A CN 113750972 B CN113750972 B CN 113750972B
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic 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
- 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 application belongs to the technical field of water treatment, and particularly provides a chromium ion adsorbent and a preparation method thereof, wherein the preparation method comprises the following steps: dopamine is treated with an amino compound. The adsorbent provided by the application has the form of nano particles, when the initial concentration of the adsorbent is 50.0mg/L of hexavalent chromium solution, the concentration of hexavalent chromium in a water sample after adsorption equilibrium is lower than 0.05mg/L, the total chromium concentration is lower than 1.5mg/L, and the removal rate is more than 95%.
Description
Technical Field
The application belongs to the technical field of water treatment, and particularly relates to a mussel-like nanoparticle-level chromium ion adsorbent, a preparation method thereof and a chromium ion adsorption method.
Background
Water pollution is one of the world's problems and is becoming a major cause of many biological deaths and diseases in the world. It is estimated that 14000 people are lost each day, with about 580 people dying from water pollution related diseases in india each day. In China, about nine of the water resources are contaminated. Thus, developing countries are faced with serious water pollution problems, and developed countries are no exception. For example, the number of the cells to be processed, the latest water report in the united states reports that 44% streams, 64% lakes, and 30% rivers have been contaminated. In recent years, along with the rapid development of industrialization, the discharge amount of chromium-containing wastewater is increased, and the wastewater seriously damages the ecological environment and influences the physical health of human bodies, so that the treatment of the chromium-containing wastewater is unprecedented.
Chromium is a very hazardous environmental pollutant, often in the form of Cr (III) and Cr (VI), an acute carcinogen, with toxicity far higher than Cr (III). Chromium and its compounds are widely used in the industrial fields of electroplating, metallurgy, tanning, metal processing, wood preservation, paint and pigment production, etc., which produce a large amount of chromium-containing waste water which is easily absorbed by the human body through the food chain and causes carcinogenesis and teratogenesis and mutation when the human body inhales excessive. If the wastewater is directly discharged without treatment, the water environment is seriously polluted.
At present, the main methods for removing chromium in wastewater are as follows: ion exchange, membrane separation, oxidation/precipitation, adsorption, etc. The adsorption method has the advantages of good adsorption effect, recycling, low cost, simple operation and the like, and is widely applied.
Currently, adsorption materials for chromium include hydrated manganese dioxide, goethite, dolomite, titanium dioxide, molecular sieves, montmorillonite, chitosan, and the like; the composite adsorbent has rice hull based mesoporous SiO 2 Cerium/ferroferric oxide, magnetic modified zeolite, diatomite-loaded ferric oxide, magnetic chitosan, graphene oxide modified biochar and the like. In the prior art, the adsorption capacity of the pure organic adsorbent is not ideal, and the adsorption effect needs to be further improved.
Disclosure of Invention
In order to solve the problems, the application discloses an adsorbent for effectively treating Cr (VI) heavy metal wastewater pollution and a sewage treatment method.
The embodiment of the application provides a method for preparing a chromium ion adsorbent, which comprises the steps of treating dopamine by utilizing an amino compound, mixing and stirring to prepare the adsorbent, wherein the amino compound is one or more of triaminoethylamine, triethylene tetramine, oxalic acid, ornithine, L-citrulline, L-arginine, leunamide, glycinamide, thiocarbamide and semicarbazide hydrochloride.
Preferably, the amino compound during the treatment is a triaminothyl amine, the ratio of the triaminothyl amine to the dopamine being 5:1 to 1:5ml/g.
Preferably, the treatment is performed in Tris buffer or dilute aqueous ammonia solution.
In another aspect, the embodiment of the application provides a chromium ion adsorbent, which is prepared by the method and is used for adsorbing hexavalent chromium ions.
Preferably, the adsorbent is a nanoparticle.
The embodiment of the application also provides a chromium ion adsorption device which comprises the chromium ion adsorbent, wherein the adsorbent can be attached to a net-shaped or sheet-shaped or tubular substrate.
In another aspect, the present application provides a method for removing chromium ions in sewage, which includes the step of adding the chromium ion adsorbent to sewage, wherein the chromium ions include, but are not limited to hexavalent chromium ions.
The embodiment of the application provides a preparation method of mussel-like nano-particles by modifying polydopamine with Dopamine (DA) serving as a main raw material at normal temperature and normal pressure and by using triaminoethylamine.
The application provides a preparation method of a mussel-like nanoparticle serving as an adsorption material with a large adsorption capacity on chromium. When the mussel-like nano particles prepared by the method adsorb hexavalent chromium solution with initial concentration of 50.0mg/L, the concentration of hexavalent chromium in a water sample after adsorption balance is lower than 0.05mg/L, the total chromium concentration is lower than 1.5mg/L, the removal rate is over 95 percent, and the total chromium content in the adsorption balance solution reaches the national comprehensive sewage discharge standard (GB 8978-1996).
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present application.
Fig. 1 is an SEM image of a mussel-like nanoparticle adsorbent prepared according to an embodiment of the present application.
Fig. 2 is a zero-point potential diagram of the mussel-like nanoparticle adsorbent prepared in the example of the present application.
FIG. 3 is a graph showing the ultraviolet contrast of the simulated mussel nanoparticle adsorbent prepared in the embodiment of the application before and after chromium adsorption.
FIG. 4 is a graph showing the removal rate and adsorption amount of Cr (VI) under different pH conditions of the mussel-like nanoparticle adsorbent prepared in the example of the present application.
FIG. 5 is a graph showing the removal rate and adsorption amount of Cr (VI) under different time conditions for the mussel-like nanoparticle adsorbent prepared in the example of the present application.
FIG. 6 is a graph showing the removal rate and adsorption amount of Cr (VI) under different concentration conditions of the mussel-like nanoparticle adsorbent prepared by the embodiment of the application.
FIG. 7 shows the results of the adsorption test of Cr (VI) after regeneration of the mussel-like nanoparticle adsorbent prepared in the example of the present application.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the application is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
The embodiment of the application provides a preparation method of a chromium ion adsorbent, which comprises the following steps: the adsorbent is prepared by treating Dopamine (DA) with an amino compound. Preferably, the amino compound is one or more of tri (2-aminoethyl) amine, tri (ethylene) amine, oxamic acid, ornithine, L-citrulline, L-arginine, leunamide, glycinamide, thiocarbamide and semicarbazide hydrochloride.
Preferably, the treatment is carried out in Tris buffer or dilute ammonia solution (concentration less than 10.5%). Further preferably, the ratio of the triaminoethylamine to the dopamine in the above treatment is 5:1 to 1:5ml/g.
Preferably, the above preparation method further comprises the step of washing the adsorbent with clean water and centrifuging.
In another aspect, the embodiment of the application provides the chromium ion adsorbent prepared by the method, wherein the chromium ion adsorbent is used for adsorbing hexavalent chromium ions.
In another aspect, the embodiment of the application also provides a method for removing chromium ions in sewage, which comprises the step of adding the chromium ion adsorbent into sewage, wherein the chromium ions are hexavalent chromium ions.
Preferably, the chromium ion adsorbent is a nanoparticle.
DA is one of the major components of the adhesion proteins secreted by the common coastal organism mussels. In weakly basic aqueous solutions, DA can form a very viscous Polydopamine (PDA) layer by air oxidation and self-aggregation at room temperature. The PDA surface is rich in active groups such as amino, imine, phenolic hydroxyl and the like, and heavy metal ions can be adsorbed through coordination, chelation, reduction and the like, so that the deep purification of heavy metals in water is realized.
As PDA is the main component of the adhesive protein secreted by marine mussel organisms, the adhesive protein has good stability, water dispersibility and biocompatibility, and functional groups such as amino groups, catechol, benzoquinone and the like in the skeleton provide a large number of active sites, heavy metals in sewage can be removed by chelation, electrostatic adsorption, reduction and the like, and Michael addition or Schiff base reaction can be carried out with specific materials containing mercapto groups and amino groups, so that the adhesive protein is fixed on the surface of the PDA to achieve the purpose of functional modification. PDA is increasingly used in biomedical, environmental protection, catalysis and other fields due to simple preparation method and mild reaction conditions.
In the embodiment of the application, the simulated mussel nano-particles are prepared by combining dopamine and triaminoethylamine and are used as chromium ion adsorbents, and the generated nano-particles have positively charged ammonium ion groups (NH) 4 + ) The positive charge of the group can attract the negative charge of the anionic heavy metal oxide, and the PDA (polydopamine) surface has a large amount of amino (-NH) 2 ) Hydroxyl (-OH) functional groups, which can be combined or reacted with heavy metal ions Cr (VI) to remove Cr (VI) from sewage and reduce it to be more toxicThe prepared adsorbent has a good adsorption/treatment effect on heavy metal Cr (VI) under the action of low Cr (III).
In the embodiment of the application, dopamine is used as a reactant, so that negative effects caused by aggregation of polydopamine are avoided. After addition of dopamine monomers, polydopamine is spontaneously formed.
In the embodiment of the application, dopamine DA is used as a main raw material, and the dopamine (and the spontaneously formed polydopamine thereof) is modified by the triaminoethylamine at normal temperature and normal pressure to prepare the mussel-like nano-particles.
The application provides a preparation method of a mussel-like nanoparticle serving as an adsorption material with a large adsorption capacity on chromium. When the mussel-like nano particles prepared by the method adsorb hexavalent chromium solution with initial concentration of 50.0mg/L, the concentration of hexavalent chromium in a water sample after adsorption balance is lower than 0.05mg/L, the total chromium concentration is lower than 1.5mg/L, the removal rate is over 95 percent, and the total chromium content in the adsorption balance solution reaches the national comprehensive sewage discharge standard (GB 8978-1996).
In specific application, the mussel-like nanoparticles can be attached to a net-shaped or sheet-shaped substrate for use, such as a metal net or a silicon wafer, so as to facilitate collection and arrangement of the nanoparticles. In one embodiment, the nano particles can be attached to the inside of the pipeline and uniformly distributed, so that the water to be treated flows into the pipeline and is adsorbed, and the treated pipeline flows out from the other end, so that the adsorption is completed.
On the other hand, the mussel-like nano-particles can be recycled and can be simply regenerated. The nanoparticles are then soaked in a high salt concentration aqueous solution, for example, 1-5 hours, to regenerate. The high salt concentration aqueous solution refers to saturated or nearly saturated aqueous solutions of sodium chloride, potassium chloride and the like.
The application is further described below by means of specific examples.
Example 1:
(1) 200mL of Tris (hydroxymethyl) aminomethane (Tris) buffer at a concentration of 0.1mol/L was added to a 500mL round bottom flask followed by 0.25mL of a solution of Triaminoethylamine (TREN).
(2) 0.25g of Dopamine (DA) was weighed out in 10mL of deionized water and added to the round bottom flask in step (1).
(3) And (3) placing a magnetic stirrer, and stirring for 24 hours in an air environment to obtain the nanoparticle mixed solution.
(4) And centrifuging the nanoparticle mixed solution by using a centrifugal machine, washing the nanoparticle mixed solution with ultrapure water for multiple times until the nanoparticle mixed solution is colorless, and centrifuging the nanoparticle mixed solution again to obtain a black solid target product, namely the mussel-like nanoparticle. Analyzing morphology of the simulated mussel nanoparticle adsorbent by using a field emission scanning electron microscope (SEM, HITACHI SU8010, japan), wherein the scanning result is shown in figure 1; the surface potential of the material was measured by using a Zetasizer Pro nano particle size and potential analyzer, and the result is shown in FIG. 2.
(5) 5mg of the mussel-like nanoparticle adsorbent was weighed and placed in 50ml of solutions containing Cr (VI) at concentrations of 50, 75, 100, 125, 150 and 200mg/L, respectively. After carrying out the shaking reaction for 48 hours at pH values of 3, 4, 5, 6 and 7 at a temperature of 25 ℃ and a rotation speed of 150 rpm, the solution was filtered with a 0.45um filter membrane, and the residual Cr (VI) concentration in the solution was measured with an ultraviolet spectrophotometer to examine the adsorption capacity.
The experimental detection results are shown in fig. 3-6, wherein fig. 3 is an ultraviolet comparison chart of the simulated mussel nanoparticle adsorbent prepared in the embodiment before and after chromium ion adsorption, and it can be seen from the chart that the absorbance difference is the largest in the wavelength range between 340 nm and 360 nm.
FIG. 4 shows the results of the detection of Cr (VI) removal rate and adsorption amount of the mussel-like nanoparticle adsorbent prepared in the above example under different pH conditions, wherein the optimal pH value is 3, and the removal rate and adsorption amount are correspondingly reduced with the increase of the pH value. The removal rate is greater than 90% at ph=3, and the adsorption amount is close to 1000mg/g. It can be seen that the mussel-like nanoparticle adsorbent prepared in this example has good Cr (VI) removal capacity at ph=3.
FIG. 5 shows the results of the detection of Cr (VI) removal rate and adsorption amount of the mussel-like nanoparticle adsorbent prepared in the above example under different time conditions. As shown, the adsorption amount reached a peak in 900 minutes (15 hours).
FIG. 6 shows the results of the detection of Cr (VI) removal rate and adsorption amount of the mussel-like nanoparticle adsorbent prepared in the above example under different concentration conditions. As shown in the figure, the removal rate of chromium ions by the adsorbent is slightly reduced with the increase of the concentration of chromium ions, but the total adsorption amount is remarkably improved, and in the concentration of 50mg/L, the adsorption amount is about one third of that under the condition of 200 mg/L. This indicates that the adsorption potential of the adsorbents provided by the present application is great.
FIG. 7 shows the adsorption amount of the simulated mussel nanoparticle adsorbent prepared in the above example, regenerated after adsorption saturation, and re-adsorbed Cr (VI) under the same conditions. As can be seen from the figure, the overall adsorption amount was decreasing with increasing number of regenerations, but the decrease was not large (about 13% decrease in the first regeneration), and the adsorption value was still higher than 1 kilo after the third regeneration.
Example 2
200mL of an aqueous ammonia solution having a concentration of 0.5% was taken and 5mL of glycinamide was added to mix. 1g of dopamine is weighed and dissolved in 10mL of deionized water, added into the mixed solution, stirred for 16 hours, centrifuged, and washed for multiple times until colorless, thus obtaining the target nanoparticle mixed solution.
The process is simple and easy to operate, and the prepared adsorbent has a good adsorption effect on Cr (VI) and can be widely applied to the advanced treatment of wastewater containing chromium and the like. And the method has simple and convenient operation for purifying the sewage containing chromium ions and high adsorption efficiency.
The adsorption capacity of the adsorbent is also compared with that of other adsorbents in the prior art, and the comparison result is shown in table 1.
Wherein table 1 shows the comparison of the adsorption effect of the simulated mussel nanoparticle adsorbent prepared in example 1 of the present application and the modified dopamine material in the prior art on Cr (VI), wherein the reaction temperature is 25 ℃.
TABLE 1 comparison of adsorption detection results
As shown by the comparison experiment, the maximum adsorption quantity of hexavalent chromium ions of the nanoparticle adsorbent prepared by the application is 7 times of that of polydopamine modified cinder and 20 times of that of polydopamine/bentonite under the same experimental conditions.
The nanoparticles prepared in example 2 were also tested as described above, with similar results to those of example 1.
The above description is only of the preferred embodiments of the present application and is not intended to limit the application, but any modifications, equivalents, improvements, etc. within the principles of the present application should be included in the scope of the present application.
Claims (6)
1. A method of preparing a chromium ion adsorbent comprising: the method comprises the steps of treating dopamine by using an amino compound, mixing and stirring to obtain the adsorbent, wherein the amino compound is triaminoethylamine, and the treatment is carried out in Tris buffer solution.
2. The method of claim 1, wherein during said treatment, the ratio of said triaminoethylamine to dopamine is 5:1 to 1:5ml/g.
3. The method of claim 1, further comprising the steps of washing the adsorbent with clean water and centrifuging.
4. A chromium ion adsorbent prepared by the method of any one of claims 1-3 and used for adsorbing hexavalent chromium ions.
5. The chromium-ion adsorbent of claim 4, wherein the chromium-ion adsorbent is a nanoparticle.
6. A method for removing chromium ions in sewage, comprising: adding the chromium ion adsorbent of claim 4 or 5 to the wastewater, wherein the chromium ions comprise hexavalent chromium ions.
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| CN114467541B (en) * | 2022-01-26 | 2023-05-02 | 西北农林科技大学 | Application of dopamine in improving heavy metal stress resistance of plants |
| CN115608392B (en) * | 2022-08-05 | 2024-02-02 | 广东工业大学 | Persulfate catalytic material and preparation method and application thereof |
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