CN115634664A - Preparation method of iron-copper modified biochar composite adsorbent and application of iron-copper modified biochar composite adsorbent in water treatment - Google Patents
Preparation method of iron-copper modified biochar composite adsorbent and application of iron-copper modified biochar composite adsorbent in water treatment Download PDFInfo
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- IYRDVAUFQZOLSB-UHFFFAOYSA-N copper iron Chemical compound [Fe].[Cu] IYRDVAUFQZOLSB-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000003463 adsorbent Substances 0.000 title claims abstract description 25
- 239000002131 composite material Substances 0.000 title claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 229960002328 chloroquine phosphate Drugs 0.000 claims abstract description 32
- AEUAEICGCMSYCQ-UHFFFAOYSA-N 4-n-(7-chloroquinolin-1-ium-4-yl)-1-n,1-n-diethylpentane-1,4-diamine;dihydrogen phosphate Chemical compound OP(O)(O)=O.ClC1=CC=C2C(NC(C)CCCN(CC)CC)=CC=NC2=C1 AEUAEICGCMSYCQ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 31
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims abstract description 17
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims abstract description 17
- 235000005822 corn Nutrition 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000010902 straw Substances 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 150000001879 copper Chemical class 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 230000007935 neutral effect Effects 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract 3
- 238000010438 heat treatment Methods 0.000 claims abstract 2
- 239000002351 wastewater Substances 0.000 claims description 20
- 240000008042 Zea mays Species 0.000 claims description 15
- 239000010949 copper Substances 0.000 claims description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 10
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 239000002699 waste material Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 7
- 238000000197 pyrolysis Methods 0.000 claims description 7
- 238000004065 wastewater treatment Methods 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 5
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 4
- 150000002505 iron Chemical class 0.000 claims description 4
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical group O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 4
- 239000002028 Biomass Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 3
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical group Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims 2
- 238000012216 screening Methods 0.000 claims 2
- -1 chloroquine phosphate compound Chemical class 0.000 claims 1
- 229960003280 cupric chloride Drugs 0.000 claims 1
- 239000012535 impurity Substances 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 22
- 239000002243 precursor Substances 0.000 abstract description 9
- 238000001354 calcination Methods 0.000 abstract description 6
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 241000209149 Zea Species 0.000 abstract 2
- 238000004140 cleaning Methods 0.000 abstract 1
- 159000000014 iron salts Chemical class 0.000 abstract 1
- 239000012299 nitrogen atmosphere Substances 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 5
- 239000002957 persistent organic pollutant Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000002154 agricultural waste Substances 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000711573 Coronaviridae Species 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013310 covalent-organic framework Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a preparation method of an iron-copper modified magnetic biochar composite adsorbent and a water treatment application thereof. The method comprises the following steps: crushing corn straws, mixing the crushed corn straws with a mixed ethanol solution of copper salts of iron salts after passing through a 80-mesh screen in a certain proportion, and heating the mixture in a water bath at 70 ℃ until the mixture is dried to obtain a precursor; calcining the precursor for 2h at 600-800 ℃ in a nitrogen atmosphere, cleaning the calcined product to be neutral by using deionized water, and drying to obtain the iron-copper modified biochar composite adsorbent material. The method has the advantages of removal rate of more than 90% in 2h for pollutants in the chloroquine phosphate polluted water body within 100ppm, good adsorption capacity, short time, high efficiency and good application prospect.
Description
Technical Field
The invention belongs to the technical field of magnetic biochar and the field of water treatment, and particularly relates to a preparation method of iron-copper modified magnetic biochar and application of the iron-copper modified magnetic biochar in adsorption treatment of chloroquine phosphate-containing wastewater.
Background
In 2019, chloroquine phosphate (CQP) has been suggested as an important and effective clinical relief drug for coronavirus (COVID-19). However, overuse will inevitably cause irreparable damage to the entire ecosystem, constituting a considerable environmental safety problem. Until now, research on such wastewater treatment has not yet matured. Therefore, it is of great interest to develop efficient methods for removing CQP from water pollution sources, such as wastewater from hospitals and pharmaceutical factories.
Adsorption is an effective physical removal method, and has been widely applied to removal of organic pollutants in various matrixes due to the characteristics of simplicity, high efficiency, economy, environmental protection and the like (https:// www. Scientific direct. Com/science/particulate/pii/S1383522020731-b 0080). However, efficient adsorption techniques require excellent adsorbents. Many types of adsorbents have been used for adsorption, including carbon nanotubes, layered double hydroxides, covalent organic frameworks and biochar. Meanwhile, modified materials having high capacity and outstanding adsorption efficiency have been receiving much attention as adsorbents and have been the focus of attention of researchers.
Disclosure of Invention
The invention discloses a method for preparing an iron-copper modified magnetic biochar adsorbing material by a one-pot method, which is used for quickly and effectively adsorbing and removing CQP from an aqueous solution. The content of adsorption active sites and acidic functional groups can be increased by carrying out magnetic modification on the biochar, the surface polarity is enhanced, the pore structure is improved by introducing iron and copper, the biochar has good chemical stability and excellent adsorption performance, and the practical application prospect of the material is verified by the good practicability of removing CQP from a simulated wastewater sample. The modified adsorbent selected by the invention is a biochar-based material, has wide sources, simple preparation and environmental friendliness, provides a possible way for resource utilization of agricultural wastes while removing organic pollutants, and conforms to the concept of treating wastes with processes of wastes against one another. This patent has opened up a high efficiency, simple, high adsorption capacity's way for getting rid of CQP.
The invention aims to provide a preparation method of an iron-copper modified magnetic biochar composite adsorbent and application of the iron-copper modified magnetic biochar composite adsorbent in treatment of chloroquine phosphate-containing wastewater.
In a first aspect, the invention provides a preparation method of an iron-copper modified magnetic biochar composite adsorbent, which comprises the following specific steps:
step one, crushing the waste corn straw biochar raw material and sieving the crushed waste corn straw biochar raw material by a sieve, preferably a 80-mesh sieve;
step two, adding the sieved corn straw powder into absolute ethyl alcohol and uniformly stirring the mixture to obtain a mixed solution; preferably, the volume of the absolute ethyl alcohol is 100mL, and the adding amount of the corn straw powder is 1.5 to 2.5g, preferably 2g
Dissolving a certain amount of ferric chloride hexahydrate and copper chloride dihydrate in the mixed solution, stirring the mixed solution on a magnetic water bath heater at 70 ℃ until absolute ethyl alcohol is volatilized to be dry, and drying the obtained dark green mixture in a 60 ℃ drying oven to obtain a precursor;
and step four, putting the precursor obtained in the step three into a tube furnace filled with nitrogen, calcining at 600-800 ℃, washing the obtained product with deionized water for multiple times until the pH value is neutral, and putting the product into an oven for drying to obtain the iron-copper modified magnetic biochar composite adsorbent material.
Preferably, the magnetic substance supported by the magnetic charcoal in the second step is iron copper ferrite. The precursor is corn stalk powder, ferric chloride hexahydrate and copper chloride dihydrate.
Preferably, in the second step, the mass ratio of the copper salt, the iron salt and the biomass is (0.17 g-1.19 g): (0.54 g-3.78 g) 2g, preferably, the molar ratio of metal elements added Cu: fe = 1.
Preferably, the pyrolysis temperature of the four-middle tube furnace in the step is 600-800 ℃.
Preferably, the dipping and stirring time in the third step is more than or equal to 60min.
In a second aspect, the invention provides the iron-copper modified magnetic biochar composite adsorbent obtained by the preparation method.
In a third aspect, the invention provides an application of an iron-copper modified magnetic biochar composite adsorbent in treatment of chloroquine phosphate-containing wastewater, which comprises the following specific steps:
preparing chloroquine phosphate solution with a certain concentration by using deionized water, adding the iron-copper modified magnetic biochar composite adsorbent into simulated wastewater, continuously oscillating on a horizontal oscillation machine at the speed of 170rpm, sampling at fixed points according to design time, and realizing adsorption removal of chloroquine phosphate.
Preferably, the simulated wastewater has a volume of 50mL and a chloroquine phosphate concentration of 20ppm to 100ppm. The adding amount of the iron-copper modified magnetic biochar is 0.1g/L, and the reaction time is 2h.
The invention has the beneficial effects that: the invention uses the dipping pyrolysis method, the principle is simple, and the method for preparing the copper ferrite magnetic biochar by using the waste corn straws as the raw material is simple. The selected modified adsorbent is a biochar-based material, has wide sources, is simple to prepare, is environment-friendly, is a large producing country of corn straws in China, has common raw materials and low cost, provides a possible way for resource utilization of agricultural wastes while removing organic pollutants, conforms to the concept of 'treating wastes with wastes', and has certain economic benefit. The iron-copper modified magnetic biochar prepared by the invention can effectively adsorb chloroquine phosphate in water and has good application prospect for treating the wastewater; according to the invention, the biochar is subjected to magnetic modification, so that the contents of adsorption active sites and acidic functional groups can be increased, the surface polarity is enhanced, the adsorption of a polluted area is facilitated, and the adsorption effect is better.
The iron-copper modified magnetic biochar prepared by the invention has both adsorption performance and magnetic performance, and has stable and good performance. The iron-copper modified magnetic biochar prepared by the invention has good magnetism, and can realize the rapid separation of materials in an external magnetic field mode, thereby achieving the aim of thoroughly removing pollutants from the environment. The invention can also synchronously treat other organic pollutants, such as rhodamine B.
Drawings
FIG. 1 is a standard curve of chloroquine phosphate concentration of 0-20 ppm at 343.2nm ultraviolet measuring wavelength.
FIG. 2 is a graph showing the comparison of the adsorption rate of chloroquine phosphate by the iron-copper modified magnetic biochar prepared by calcination at different temperatures in example 2.
Fig. 3 is an effect diagram of adsorbing chloroquine phosphate wastewater by iron-copper modified magnetic biochar compounded in different proportions in example 3, wherein: the material A, the material B, the material C and the material D are four different groups of iron-copper modified magnetic biochar.
FIG. 4 is a graph comparing the treatment effect of the iron-copper modified magnetic biochar on chloroquine phosphate with different initial concentrations in example 4.
FIG. 5 is a graph showing the effect of iron-copper modified magnetic biochar on rhodamine B at a concentration of 20ppm in the example.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
Example 1
As shown in fig. 1, a standard curve of chloroquine phosphate on an ultraviolet spectrophotometer is configured, and the specific steps are as follows:
for generally dilute solutions, the beer-lambert law holds that the concentration of a solution solute is directly proportional to the absorbance. Selecting 343.2nm as the characteristic absorption wavelength of chloroquine phosphate, and preparing a solution with dry weight concentration of 0.5mg/L, 1mg/L, 2mg/L, 5mg/L, 10mg/L and 20mg/L to draw a chloroquine phosphate standard curve.
Example 2
In order to verify that the prepared iron-copper modified magnetic biochar can show different adsorption performances at different calcining temperatures, 2g of sieved corn straw powder is added into 100ml of absolute ethyl alcohol and is uniformly stirred to obtain a mixed solution; then, dissolving 0.05mol/L ferric chloride hexahydrate and 0.1mol/L copper chloride dihydrate in the mixed solution, stirring the solution on a magnetic water bath heater at 70 ℃ until absolute ethyl alcohol is volatilized, and putting the obtained dark green mixture into a 60 ℃ oven for drying to obtain a precursor; and putting the precursor into a tube furnace filled with nitrogen, wherein the pyrolysis temperature is set to be three groups of 600 ℃, 700 ℃ and 800 ℃, and the pyrolysis time is 2 hours. The names of the materials are denoted as material H, material G, and material A.
The treatment result of the obtained wastewater is shown in fig. 2 (in the figure, the material H, the material G and the material A are iron-copper modified magnetic biochar groups at three different calcination temperatures), and as can be seen from fig. 2, the material calcined at 800 ℃ has more excellent adsorption performance.
Example 3
In order to optimize the degradation performance of iron-copper modified magnetic biochar compounded in different proportions, the molar ratio of metal elements added in an iron-copper modified magnetic biochar precursor Cu: fe = 1; wherein, the concentration of copper element is 0.01-0.07 mol/L, the concentration of iron element is 0.02-0.14 mol/L; the rest parameters are set to be the same, the adding amount of the precursor corn straw is 2g, and the calcining temperature is set to be 800 ℃. In the figure 3, a material A (the concentration of copper element is 0.05mol/L and the concentration of iron element is 0.1 mol/L), a material B (the concentration of copper element is 0.07mol/L and the concentration of iron element is 0.14 mol/L), a material C (the concentration of copper element is 0.03mol/L and the concentration of iron element is 0.06 mol/L), a material D (the concentration of copper element is 0.01mol/L and the concentration of iron element is 0.02 mol/L) are four groups of iron-copper modified magnetic biochar groups prepared under different compounding ratios, 0.1g of the materials are added into 50ml of water samples, the wastewater samples are sampled and analyzed when the reaction time is 5min, 10min, 20min, 40min, 60min, 90min, 120min, 150min and 180min, and the initial concentration of chloroquine phosphate in simulated wastewater is 400mg/L.
The obtained wastewater treatment results are shown in FIG. 4. As can be seen from the figure, the adsorption effect of the material C (the concentration of the added copper element is 0.03mol/L and the concentration of the added iron element is 0.06 mol/L) is the best after the materials are added. The maximum theoretical equilibrium adsorption capacity is 85 mg/g.
Example 4
In order to verify the effect of the prepared iron-copper modified magnetic biochar on treatment of chloroquine phosphate-containing wastewater with different concentrations, 0.1g of the iron-copper modified magnetic biochar material C prepared in example 3 is added into 50ml of chloroquine phosphate-containing simulated wastewater with different concentrations, and sample components are sampled and analyzed when the reaction time is 5min, 10min, 20min, 40min, 60min, 90min, 120min, 150min and 180min respectively.
The obtained wastewater treatment results are shown in FIG. 4, from which it can be seen that the adsorption amount rapidly increases in the initial stage, gradually decreases after 2 hours until the adsorption is saturated, and the maximum theoretical equilibrium adsorption amount is 85 mg/g. Meanwhile, the concentrations of the wastewater simulating chloroquine phosphate with different initial concentrations are reduced after the wastewater is treated, which indicates that the iron-copper modified magnetic biochar can treat chloroquine phosphate wastewater with various concentrations, is applied to various stages of chloroquine phosphate wastewater treatment, and when the concentration is within 100ppm, the removal rate can reach more than 99% within two hours.
Example 5
In order to verify the effect of the prepared iron-copper modified magnetic biochar on treating other wastewater containing organic matters, 0.1g of iron-copper modified magnetic biochar material C prepared in example 3 is put into 50ml of simulated wastewater containing rhodamine B at the concentration of 25ppm, and samples are taken for analysis of sample components when the reaction time is 5min, 10min, 20min, 40min, 60min, 90min and 120min respectively.
The obtained wastewater treatment results are shown in FIG. 5, from which it can be seen that the removal rate rapidly increased in the initial stage and reached 99% or more after 40 mins. The invention can also synchronously treat other organic pollutants, such as rhodamine B.
Claims (10)
1. A preparation method of an iron-copper modified magnetic biochar composite adsorbent is characterized by comprising the following steps:
s1, crushing corn straws and screening the crushed corn straws by a screen;
s2, uniformly mixing the sieved corn straw powder with absolute ethyl alcohol;
s3, adding iron salt and copper salt into the mixed liquid of S2;
s4, heating the mixed liquid in a water bath at the temperature of 60-80 ℃ until the mixed liquid is dried to obtain a dark green mixture;
s5, drying the mixture at 50-70 ℃;
s6, placing the mixture obtained in the step S5 into a tubular furnace for anaerobic pyrolysis to obtain a product, washing the product with deionized water until the pH value is neutral, and drying to obtain the iron-copper modified biochar composite adsorbent material.
2. The method according to claim 1, wherein in step S1, the waste corn stalks are cleaned and air-dried, and crushed and sieved after impurities are removed; the screening mesh number of the corn straw powder is 80 meshes.
3. The method according to claim 1, wherein the volume of the absolute ethanol in the step S2 is 100mL, and the amount of the corn stalk powder added is 1.5 to 2.5g, preferably 2g.
4. The method of claim 1, wherein in step S3 the iron salt is ferric chloride hexahydrate and the copper salt is cupric chloride dihydrate.
5. The method according to claim 4, characterized in that the concentration of copper element is 0.01-0.07 mol/L and the concentration of iron element is 0.02-0.14 mol/L, preferably the molar ratio of the addition of iron and copper elements Cu: fe = 1.
6. The method of claim 1, wherein the pyrolysis temperature of the tubular furnace in the step S6 is 600-800 ℃ and the pyrolysis time is 1-3h.
7. The method of claim 1, wherein: in the step S3, the mass ratio of the copper salt to the iron salt to the biomass is 0.17-1.19 g:0.54 g-3.78g.
8. The iron-copper modified magnetic biochar composite adsorbent prepared according to the method of any one of claims 1 to 7.
9. The application of the iron-copper modified magnetic biochar composite adsorbent for chloroquine phosphate pharmaceutical wastewater treatment as claimed in claim 8, wherein the iron-copper modified magnetic biochar composite adsorbent is used for chloroquine phosphate pharmaceutical wastewater treatment, and is characterized in that: and (3) adsorbing the chloroquine phosphate compound wastewater by using a chloroquine phosphate water sample and the iron-copper modified magnetic biochar composite adsorbent.
10. Use according to claim 9, characterized in that: mixing and oscillating according to the proportion that 0.05-0.2g of adsorbent material is added into 100ml of water sample, the concentration of chloroquine phosphate is adjusted to 20-400 ppm, and the reaction time is 150-210mins.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11866349B1 (en) | 2023-09-05 | 2024-01-09 | King Faisal University | Method of chromium (CR+6) removal from wastewater using copper augmented biochar |
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