CN109107537B - Adsorbent for treating hexavalent chromium in neutral wastewater and preparation method thereof - Google Patents
Adsorbent for treating hexavalent chromium in neutral wastewater and preparation method thereof Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- C02F2101/00—Nature of the contaminant
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Abstract
The invention discloses an adsorbent for treating hexavalent chromium in neutral wastewater and a preparation method thereof, belonging to the fields of sewage treatment and environmental protection. The structural formula of the adsorbent for treating hexavalent chromium in neutral wastewater is N4O6CXH2X+1and-GO, wherein X is more than or equal to 15 and less than or equal to 37, and X is a positive integer, firstly synthesizing Graphene Oxide (GO), and then carrying out functional treatment on the graphene oxide to obtain the functionalized graphene oxide adsorbent. The prepared adsorbent has the advantages of large specific surface area, good selectivity and high adsorption efficiency, and the adsorption rate of the prepared adsorbent to Cr (VI) is more than 96% in the range of pH = 2-9. The preparation method of the adsorbent for treating hexavalent chromium in neutral wastewater provided by the invention has the advantages of low reaction temperature, short time, simplicity in purification and strong operability.
Description
Technical Field
The invention relates to an adsorbent for treating hexavalent chromium in neutral wastewater and a preparation method thereof, belonging to the industrial sewage treatment range, in particular to a method for treating wastewater containing Cr (VI) generated in the industrial production process by using a functionalized graphene oxide adsorbent under a neutral condition so as to enable the wastewater to reach the national discharge standard required by Cr (VI).
Background
With the rapid development of industry, heavy metal pollution generated in the production processes of leather making, electroplating, pigment manufacturing and the like causes great harm to the environmental balance and human health. In heavy metal pollution such as lead, mercury, cadmium, cobalt, chromium and the like, chromium is mainly applied to the fields of tanning, metallurgy, paint, printing and dyeing and the like. In nature, there are two valence states of Cr (III) and Cr (VI), and Cr (III) is an essential element for the metabolism of sugar, protein and fat. However, prolonged exposure to Cr (VI) causes respiratory inflammation and induces lung cancer or invasive skin lesions, and severe hexavalent chromium poisoning can also lead to death. Cr (VI) in solution with negatively charged HCrO4 -、Cr2O7 2−、CrO4 2−Mainly comprises the following steps. Thus, cr (vi) is predominantly in the singlet state H when the pH of the wastewater solution =2-5.5CrO4 -The presence of ions; when the pH value of the waste water solution is more than or equal to 5.5, Cr (VI) is mainly divalent CrO4 2−Ions are present. The reported optimum adsorption conditions for adsorbents are generally at pH =2-3, which is not suitable for near neutral surface waters and soils. Therefore, the method is beneficial to solving the problem of high-efficiency Cr (VI) adsorption under neutral conditions.
The traditional method for treating the wastewater containing Cr (VI) comprises a reduction precipitation method, a plant restoration method, a membrane separation method, an electrochemical method and the like. The reduction precipitation method is to add reducing agent, such as sodium sulfite, ferrous sulfate, etc. into the waste water containing Cr (VI), firstly reduce to Cr (III), then precipitate or flocculate. The phytoremediation method is to treat pollutants in the environment by utilizing the functions of absorption, metabolism, degradation and the like of plants and coexisting microorganisms thereof to the environment, but the biomass of the plants is low, the plants grow slowly, and the growth period is long, so that the remediation efficiency is low, the plants are not easy to mechanically operate, and the rotten fallen leaves can cause heavy metal pollutants to return to soil, thereby causing secondary pollution. The membrane separation method uses a special semipermeable membrane to make a solute in the solution permeate out of the solvent under the action of external pressure, so as to attain the goal of separation. However, this method is expensive in equipment and operation, and the membrane is easily clogged during operation, and thus is periodically cleaned and maintained, and a large amount of cleaning solution is consumed, thereby generating organic pollutants. The electrochemical method being Fe produced by electrolysis of iron2+Cr (VI) is reduced into Cr (III), and then neutralized and precipitated, and solid-liquid separation is carried out, although the method occupies small area, the power consumption is large, the volume of the treated wastewater is small, and the method is not suitable for large-scale popularization. Therefore, it is required to provide an adsorbent which has high adsorption efficiency, large specific surface area, wide applicable pH range and no secondary pollution.
The graphene oxide is used as a raw material, and is rich in oxygen-containing functional groups such as hydroxyl, epoxy, carboxyl, carbonyl and the like. In its functionalization, it is desirable to achieve a selective purification effect on cr (vi) under neutral conditions. Therefore, the invention provides an adsorbent for treating hexavalent chromium in neutral wastewater and a preparation method thereof.
Disclosure of Invention
Aiming at the problems of good adsorption effect under acidic condition and almost no adsorption under neutral and alkaline conditions in the prior art, the invention aims to provide the adsorbent for treating hexavalent chromium in neutral wastewater, and the prepared adsorbent has the advantages of wide pH application range, low price and easily available raw materials.
The second purpose of the invention is to provide a preparation method of the adsorbent for treating hexavalent chromium in neutral wastewater. The adsorbent prepared by the method has large specific surface area and uniform particle size distribution.
In order to achieve the purpose, the technical scheme of the invention is as follows:
an adsorbent for treating hexavalent chromium in neutral wastewater: the structure of the adsorbent is N2CXH2X+1-GO, where 9 ≦ X ≦ 29, (X is a positive integer).
The adsorbent has a specific surface area of 30m2/g-250m2The selectivity is single, and the applicable pH range is 2-9.
A preparation method of an adsorbent for treating hexavalent chromium in neutral wastewater comprises the following steps:
step one, synthesizing GO by a modified Hummer method;
secondly, reacting tetramethylmethanediamine and brominated alkane in a solvent to obtain a product I;
step three, continuing to react the product I to prepare a functional reagent I;
step four, loading a functionalized reagent I on GO in a solvent to synthesize functionalized graphene oxide;
wherein, the brominated alkanes in the second step are brominated pentane, brominated hexane, brominated heptane, brominated octane, brominated nonane, brominated decane, brominated dodecane, brominated tetradecane and brominated hexadecane;
wherein, the reaction solvent in the second step is dimethylformamide, dimethylacetamide, tetrahydrofuran and acetonitrile;
the solvent used in the fourth step is acetone, ethyl acetate and butyl acetate;
in the second step, the mass of the tetramethylmethanediamine is 1-2 g, the volume of the solvent is 3-6 mL, the mass of the bromoalkane is 4-14 g, and the reaction temperature is 55-85oC, reacting for 10-24 hours, and purifying and recrystallizing for multiple times by using ethanol-ethyl acetate with the volume ratio of 1:2-1:5 to obtain a product I;
dissolving the product I in ethyl acetate to react with 3mol/L NaOH solution, washing the product I with deionized water for many times until the product I is neutral, and continuing to react with 4mol/L HNO3Reacting, washing the reaction product with deionized water for multiple times until the reaction product is neutral to obtain a functionalized reagent I;
in the fourth step, 0.5-1g of the functionalized reagent I is dissolved in the solvent, 1-2 g of GO is dispersed in the solvent, and the reaction temperature is 15-45oC, the reaction time is 8-15 h; and centrifuging, washing and drying to obtain the functionalized graphene oxide adsorbent.
Advantageous effects
1. The adsorbent for treating hexavalent chromium in neutral wastewater is an organic-inorganic hybrid material, has low cost and can be produced in a large scale in practice; the structure and the performance are excellent, and the adsorption rate of the composite material to Cr (VI) in the environment with the pH range of 2-9 is more than 96 percent;
2. the adsorbent for treating hexavalent chromium in neutral wastewater has good regeneration performance and low desorption-regeneration cost, and can be recycled.
3. The preparation method of the adsorbent for treating hexavalent chromium in neutral wastewater has the advantages of low reaction temperature, short reaction time, simple and convenient subsequent treatment and strong operability.
Drawings
FIG. 1 is a nuclear magnetic hydrogen spectrum diagram of a functionalizing agent I prepared in example 1.
Fig. 2 is a structural diagram of a functionalized graphene oxide adsorbent prepared in example 2.
Fig. 3 is an infrared spectrum of a functionalized graphene oxide adsorbent prepared in example 2.
Detailed Description
The invention is described in detail below by means of specific examples:
the final products of examples 1-9 of the invention were tested by the following instruments and methods: analyzing the molecular structure and the product purity by a full digital nuclear magnetic resonance spectrometer (advanced III400 MHz); performing qualitative analysis on the adsorbent by using a Fourier transform infrared spectrometer (Vertex 70); measuring the specific surface area of the adsorbent by a BET type specific surface area tester (M9-3H-2000 BET-M); the content of Cr (VI) in the supernatant after adsorption was measured by an atomic absorption spectrometer (PinAcle 900T).
The final products of examples 1-5 of the present invention have the following steps of determining the adsorption rate of Cr (VI): placing 0.1 g of functionalized graphene adsorbent in an erlenmeyer flask, then adding 10 mL of solution containing 0.2 g/L of Cr (VI) and having pH =6.8, stirring at room temperature for 30 min to reach adsorption equilibrium, centrifuging to obtain supernatant, measuring the content of Cr (VI) by an atomic absorption method, and measuring the content according to a formula
(E is adsorption rate, C)OIs the initial concentration of Cr (VI), CeConcentration at adsorption equilibrium) was calculated.
Example 1
1g of tetramethylmethanediamine, 5.5 g of bromododecane, 3 mL of dimethylformamide as a solvent, and a reaction temperature of 80oC, reaction time is 12 h; recrystallizing with ethanol-ethyl acetate for three times to obtain a product I; dissolving the product I in ethyl acetate and 20 mL of 3mol/L NaOH solution for reaction, and washing the product I to be neutral by deionized water for multiple times; continuing with 20 mL of 4mol/L HNO3Reacting, washing the reaction product with deionized water for multiple times until the reaction product is neutral to obtain a functionalized reagent I with the mass of 5.1 g; the structure was determined by nuclear magnetic assay (see FIG. 1).
Example 2
0.5 g of the functionalizing agent I is dissolved in acetone, 1g of GO is ultrasonically dispersed in the acetone, and 25 g of the functionalizing agent I is dissolved in the acetoneoC stirring and reacting for 10 hours, centrifuging, washing with deionized water, and 60oAnd C, drying in vacuum for 12 h to obtain a functionalized graphene oxide I adsorbent, successfully detecting and loading by infrared (see attached figure 3), and calculating according to the method that the adsorption rate of Cr (VI) at pH =2-9 is greater than 96%, wherein the adsorption rate is shown in the following table:
| pH | 2.3 | 3.4 | 4.6 | 5.5 | 6.4 | 7.7 | 8.6 |
| E(100%) | 97.4 | 97.1 | 97.6 | 97.2 | 97.9 | 98.0 | 97.4 |
example 3
1g of tetramethylmethanediamine, 4.3 g of bromoheptane and 4 mL of acetonitrile as solvents, wherein the reaction temperature is 75oC, reaction time is 10 h; recrystallizing with ethanol-ethyl acetate for three times to obtain a product II; dissolving the product II in ethyl acetate and 20 mL of 3mol/L NaOH solution for reaction, and washing the product II to be neutral by deionized water for multiple times; continuing with 20 mL of 4mol/L HNO3Reacting, washing with deionized water for many times to neutrality to obtain a functionalized reagent IIThe amount was 3.2 g; 0.5 g of the functionalizing agent II is dissolved in acetone, 1.0 g of GO is ultrasonically dispersed in the acetone, and 30 g of the functionalizing agent IIoC stirring and reacting for 12 h, centrifuging, washing with deionized water, and 60oAnd C, drying in vacuum for 12 h to obtain the functionalized graphene oxide II adsorbent, and calculating according to the method to obtain the adsorption rate of Cr (VI) of 97.2%.
Example 4
1g of tetramethylmethanediamine, 4.8 g of bromononane and 4 mL of dimethylacetamide as a solvent, and the reaction temperature is 65oC, reaction time is 12 h; recrystallizing with ethanol-ethyl acetate for three times to obtain a product III; dissolving the product III in ethyl acetate and 20 mL of 3mol/L NaOH solution for reaction, and washing the product III with deionized water for multiple times until the product is neutral; continuing with 20 mL of 4mol/L HNO3Reacting, washing the reaction product with deionized water for multiple times until the reaction product is neutral to obtain a functionalized reagent II with the mass of 3.4 g; 0.5 g of the functionalized reagent III is dissolved in butyl acetate, 1.0 g of GO is dispersed in the butyl acetate by ultrasonic, 28 g of the functionalized reagent IIIoC stirring and reacting for 10 hours, centrifuging, washing with deionized water, and 60oAnd C, drying in vacuum for 12 h to obtain the functionalized graphene oxide III adsorbent, and calculating according to the method to obtain the adsorption rate of Cr (VI) of 97.9%.
Example 5
1g of tetramethylmethanediamine, 5.4 g of bromodecane and 5 mL of tetrahydrofuran as solvents, and the reaction temperature is 70oC, reaction time is 10 h; recrystallizing with ethanol-ethyl acetate for three times to obtain a product IV; dissolving the product IV in ethyl acetate and 20 mL of 3mol/L NaOH solution for reaction, and washing the product IV with deionized water for multiple times until the product is neutral; continuing with 20 mL of 4mol/L HNO3Reacting, washing the reaction product with deionized water for multiple times until the reaction product is neutral to obtain a functionalized reagent IV with the mass of 3.4 g; 0.5 g of the functionalized reagent III is dissolved in butyl acetate, 1.0 g of GO is dispersed in the butyl acetate by ultrasonic, 28 g of the functionalized reagent IIIoC stirring and reacting for 10 hours, centrifuging, washing with deionized water, and 60oAnd C, drying in vacuum for 12 h to obtain the functionalized graphene oxide IV adsorbent, and calculating according to the method to obtain the adsorption rate of Cr (VI) of 96.7%.
Example 6
Taking 10 mL of 0.2 g/L solution containing Cr (VI), adding 0.2 g of KCl and KNO3、KCO3、K2SO4、K3PO4Adjusting the pH =6.5 of the solution, adding 0.1 g of functionalized graphene oxide I adsorbent, stirring at room temperature for 30 minutes to reach adsorption equilibrium, centrifuging, taking supernate, measuring the content of Cr (VI) by using an atomic absorption method, and calculating the adsorption rate of Cr (VI) to be 96.3%.
Example 7
Taking 10 mL of 0.2 g/L Cr (VI) -containing solution, adding 0.3 ZnCl2、CoCl2、CuCl2、NiCl2、CdCl2、MgCl2Adjusting the pH =6.9 of the solution, adding 0.1 g of functionalized graphene oxide I adsorbent, stirring at room temperature for 30 minutes to reach adsorption equilibrium, centrifuging, taking supernate, measuring the content of Cr (VI) by using an atomic absorption method, and calculating the adsorption rate of Cr (VI) to be 96.7%.
Claims (3)
1. An adsorbent for treating hexavalent chromium in neutral wastewater, which is characterized in that the structure of the adsorbent is N4O6CXH2X+1-GO, wherein X is more than or equal to 15 and less than or equal to 37, X is a positive integer, and the preparation method comprises the following steps:
step one, synthesizing GO by a modified Hummer method;
secondly, reacting tetramethylmethanediamine and brominated alkane in a solvent to obtain a product 1;
step three, continuously reacting the product 1 to prepare a functional reagent I;
step four, loading a functional reagent on GO in a solvent to synthesize a functional graphene oxide adsorbent;
wherein the brominated alkane in the second step is one or more of brominated pentane, brominated hexane, brominated heptane, brominated octane, brominated nonane, brominated decane, brominated dodecane, brominated tetradecane and brominated hexadecane; in the second step, the reaction solvent is one or more of dimethylformamide, dimethylacetamide, tetrahydrofuran and acetonitrile;
the solvent used in the fourth step is one or more of acetone, acetonitrile, ethyl acetate and butyl acetate, the mass of the tetramethylmethanediamine in the second step is 1-2 g, the volume of the solvent is 3-6 mL, the mass of the brominated alkane is 4-14 g, and the reaction temperature is 55-85oC, the reaction time is 10 to 24h, purifying and recrystallizing for multiple times by using ethanol-ethyl acetate with the volume ratio of 1:2-1:5 to obtain a product 1; dissolving the product 1 in ethyl acetate to react with 3mol/L NaOH solution, washing the product with deionized water for many times until the product is neutral, and continuing to react with 4mol/L HNO3Reacting, washing with deionized water for many times until the reaction is neutral, and obtaining the functionalized reagent I.
2. The adsorbent for treating hexavalent chromium in neutral wastewater according to claim 1, wherein: the adsorbent has a specific surface area of 30m2/g-250m2The applicable pH range is 2-9.
3. The adsorbent for treating hexavalent chromium in neutral wastewater according to claim 1, wherein: in the fourth step, 0.5-1g of the functionalized reagent I is dissolved in the solvent, 1-2 g of GO is dispersed in the solvent, and the reaction temperature is 15-45oC, the reaction time is 8-15 h; and centrifuging, washing and drying to obtain the functionalized graphene oxide adsorbent.
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| CN111790359A (en) * | 2020-06-18 | 2020-10-20 | 济南大学 | Adsorbent for treating hexavalent chromium in wastewater |
| CN111644162A (en) * | 2020-06-18 | 2020-09-11 | 济南大学 | Adsorbent for treating hexavalent molybdenum in alkaline wastewater |
| CN113318710A (en) * | 2021-07-07 | 2021-08-31 | 长春工业大学 | Preparation method of graphene oxide/chitosan composite material adsorbent |
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