CN112473626A - Cellulose-based composite adsorbent for wastewater treatment - Google Patents
Cellulose-based composite adsorbent for wastewater treatment Download PDFInfo
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses a cellulose-based composite adsorbent for wastewater treatment, and relates to the technical field of adsorbents for wastewater treatment. The preparation method of the cellulose-based composite adsorbent comprises the following steps: bagasse pretreatment, namely separating, purifying and crushing bagasse raw materials, and then carrying out ultrasonic-alkali liquor-ultrasonic combined pretreatment to generate alkali fibers; chemically modifying, namely oxidizing the alkali fiber by adopting sodium perchlorate to obtain oxidized fiber; placing the oxidized fiber in a reaction medium, adding acid anhydride for reaction, washing, dipping, filtering and drying, and then carrying out esterification reaction with guanosine to obtain a product A; and putting the product A into a diaminopimelic acid aqueous solution for constant-temperature reaction, and then washing and drying to obtain the cellulose-based composite adsorbent. The cellulose-based composite adsorbent for wastewater treatment, which is prepared by the invention, has higher adsorption performance and better removal effect on heavy metal ions and printing and dyeing waste in wastewater; and the method can be recycled, is simple to operate and has high adsorption efficiency.
Description
Technical Field
The invention belongs to the technical field of adsorbents for wastewater treatment, and particularly relates to a cellulose-based composite adsorbent for wastewater treatment.
Background
With the development of industrialization and the growth of population, a large amount of industrial and domestic waste is generated, so that more and more water sources are polluted. The most common pollution in surface water in China is organic pollution, heavy metal pollution, eutrophic pollution, composite pollution and the like. The problem of water pollution becomes an important factor for restricting economic development and harming human health, and the requirement on environmental protection is more and more strong along with the development and transformation upgrade of economy in China, so that the development and application of a novel non-toxic and harmless water treatment agent becomes a research hotspot for water pollution treatment at present.
The adsorption method is an effective method for removing pollutants in water by utilizing a unique physical structure or functional groups of the adsorbent through physical adsorption, chemical adsorption or physical-chemical comprehensive adsorption, is suitable for treating heavy metal wastewater with lower concentration, and also has a good decoloration effect on dye wastewater. The adsorption method has the advantages of wide application range, no secondary pollution and the like, thereby being widely applied to wastewater treatment. The adsorbents are various, currently, activated carbon, bentonite, synthetic fibers, high polymers and the like are commonly used, and many of the materials are non-renewable or non-biodegradable, so that the production cost is high or secondary pollution is caused. With the emphasis on ecological safety and green chemistry, people hope to find nontoxic, harmless, safe and stable adsorbents, so that the development and utilization of biomass adsorbents rich in resources in nature become research hotspots of many researchers at home and abroad.
Cellulose is a natural polymer which is widely distributed and most abundant in nature, and is a basic substance for forming plant cell walls. Annually, plants produce billions of tons of cellulose through photosynthesis, a renewable resource that is inexhaustible. Cellulose is macromolecular polysaccharide formed by connecting D-glucose with beta-1, 4 glycosidic bonds, and the cellulose can be used as an adsorbing material due to a large amount of hydroxyl, but the single cellulose molecule has weak adsorption capacity, and the cellulose can be used as an adsorbing material with good performance only by chemically modifying the cellulose molecule to have more or stronger adsorption groups.
Disclosure of Invention
The invention aims to provide a cellulose-based composite adsorbent for wastewater treatment, which has high adsorption performance and has good adsorption effect on heavy metal ions and printing and dyeing waste in wastewater; and can be recycled.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a method for preparing a cellulose-based composite adsorbent for wastewater treatment, comprising:
s1: bagasse pretreatment, namely separating, purifying and crushing bagasse raw materials, and then carrying out ultrasonic-alkali liquor-ultrasonic combined pretreatment to generate alkali fibers;
s2: chemically modifying, namely oxidizing the alkali fiber by adopting sodium perchlorate to obtain oxidized fiber;
placing the oxidized fiber in a pyridine or N, N-dimethylacetamide reflux medium, adding acid anhydride for reaction, washing, soaking, filtering, drying, and performing esterification reaction with guanosine to obtain a product A;
and (3) putting the product A into a diaminopimelic acid aqueous solution for constant-temperature reaction, and then washing and drying to obtain the cellulose-based composite adsorbent. Bagasse is a byproduct in sugar manufacturing industry, the main components are cellulose, lignin, hemicellulose, ash, crude protein and the like, the bagasse is a biomass material with wide resources and low price, and a large amount of hemicellulose and lignin are removed after pretreatment, so that the sheet structure of the bagasse is damaged, and the fibers are separated and thinned; after chemical modification, new functional groups are given to the bagasse, amino, imino, ester and carboxyl are introduced into the side chain of the bagasse to prepare a zwitterionic adsorbent, and the adsorption capacity of the bagasse on heavy metal ions and organic pollutants is improved through the actions of ion exchange, electrostatic attraction, van der Waals force, hydrogen bonds, surface adsorption and the like, so that the purpose of removing pollutants is achieved; meanwhile, the interior of the bagasse is loosened, the number of holes in the structure of the bagasse can be increased, the diameter of the holes is reduced, the surface of the material becomes rough, folds and grooves appear, the adsorption effect of the composite material is enhanced, and the adsorption efficiency is better; in addition, the biomass resources can be efficiently utilized through recycling. The adsorbent prepared by chemically modifying cellulose has good adsorption capacity on both anionic pollutants and cationic pollutants in wastewater, and can be used for purification treatment of industrial heavy metal ion wastewater and dye wastewater.
Preferably, the chemical modification gives a material having the formula:
Preferably, the mass ratio of the oxidized cellulose to the acid anhydride to the guanosine and the diaminopimelic acid is 1: 5-6: 5.5-6.5: 10 to 12.
Preferably, the specific oxidation treatment process in step S2 is: the concentration of the sodium periodate aqueous solution is 10-12 g/L, and the solid-to-liquid ratio of the alkali cellulose to the sodium periodate aqueous solution is 1: 40-48 g/mL; the temperature reaction is 40-50 ℃, and the reaction time is 3-4 h; after the reaction is finished, the cellulose base is filtered off, washed to neutrality and dried in vacuum.
Preferably, the esterification reaction in step S2 is specifically prepared by:
dissolving guanosine in DMF, adding EDC and DMAP (the mass ratio of EDC to DMAP to guanosine is 1: 0.2-0.3: 1.4-1.5), stirring for 15min, adding the cellulose modified by anhydride, and continuously stirring for reacting for 46-48 h. Pouring the reaction product into water, extracting with ethyl acetate, washing with saturated sodium bicarbonate solution and saturated brine respectively, drying the organic phase with anhydrous sodium sulfate overnight, filtering, separating by silica gel column chromatography (eluent is ethyl acetate and petroleum ether with the volume ratio of 1: 2-3), distilling under reduced pressure, and drying under vacuum to obtain the product A.
Preferably, the acid anhydride in step S2 is one of succinic anhydride, maleic anhydride, and acetic anhydride.
Preferably, the solid-to-liquid ratio of the oxidized fibers to the medium in step S2 is 1: 20-25 g/mL.
Preferably, the sericite powder is added after the chemical modification, and the cellulose-based composite adsorbent is obtained after the uniform stirring, mixing and drying; wherein the mass ratio of the sericite powder to the oxidized cellulose is 1: 2 to 3. Sericite powder belongs to silicate minerals with a layered structure, is rich in elasticity, can be bent, and has good abrasion resistance and wear resistance and stable chemical properties. The sericite powder is added, so that the cellulose crystal structure can be promoted to be changed from a cellulose I structure to a cellulose II structure, and the surface adsorption effect of the composite material is enhanced; particularly, the adsorption performance of the composite material to heavy metal ions is enhanced; and the porosity of the cellulose-based adsorbent can be improved, the time for reaching adsorption balance is reduced, and the adsorption efficiency of the adsorbent is improved.
The invention also aims to disclose a cellulose-based composite adsorbent for wastewater treatment.
Preferably, the adsorbent has an adsorption capacity of > 160mg/g for heavy metal ions. More preferably, the adsorbent is for Cu2+The adsorption capacity of the adsorbent is more than 180 mg/g; adsorbent pair Pb2+The adsorption capacity of (A) is more than 160 mg/g.
Preferably, the adsorption capacity for the dye is > 200 mg/g. More preferably, the adsorbent has an adsorption capacity of > 270mg/g for CR; the adsorption capacity of the adsorbent to MB is more than 200 mg/g.
The invention also discloses application of the cellulose-based composite adsorbent for wastewater treatment in the field of wastewater treatment.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, cellulose is extracted from bagasse, and is chemically modified to introduce amino, imino, ester and carboxyl functional groups, so that the prepared cellulose-based composite adsorbent can improve the adsorption capacity of the bagasse on heavy metal ions and organic pollutants in wastewater through the actions of ion exchange, electrostatic attraction, van der Waals force, hydrogen bonds, surface adsorption and the like, and the purpose of removing pollutants is achieved; in addition, the efficient utilization of biomass resources is realized. After the sericite powder is added, the porosity of the cellulose-based adsorbent can be improved, the cellulose crystal structure is promoted to be changed from a cellulose I structure to a cellulose II structure, the surface adsorption effect of the composite material is enhanced, and the adsorption performance of the composite material on metal ions is further enhanced; and the time for reaching adsorption balance can be reduced, and the adsorption efficiency is improved.
Therefore, the invention provides a cellulose-based composite adsorbent for wastewater treatment, which has high adsorption performance and good adsorption effect on heavy metal ions and printing and dyeing waste in wastewater; and can be recycled.
Drawings
FIG. 1 is a schematic diagram of XPS spectrum-broad spectrum in test example 1 of the present invention;
FIG. 2 is a XPS spectrum-high resolution C1s peak spectrum diagram in test example 1 of the present invention;
FIG. 3 is a graph showing the results of the adsorption capacity test in test example 2 of the present invention;
FIG. 4 is a graph showing the comparison of the results of the adsorption rate test in test example 2 of the present invention;
FIG. 5 is a graph showing the results of the recycling test in test example 2 of the present invention.
Detailed Description
The technical solution of the present invention is further described in detail below with reference to the following detailed description and the accompanying drawings:
example 1:
preparation of cellulose-based composite adsorbent for wastewater treatment:
s1: bagasse pretreatment, namely removing impurities from bagasse raw materials, adding the bagasse raw materials into a sodium hydroxide solution with the mass fraction of 3%, boiling for 20min, washing with water, drying and shearing; then carrying out ultrasonic wave-alkali liquor-ultrasonic wave combined pretreatment: dispersing bagasse in water, and controlling a solid-liquid ratio to be 1: 30g/mL, and then carrying out ultrasonic treatment for 15 min; and (3) after filtering, putting the mixture into a sodium hydroxide solution with the mass fraction of 10%, and boiling for 60min, wherein the solid-liquid ratio is controlled to be 1: continuing ultrasonic treatment for 30min at a concentration of 30g/mL, filtering, washing with water to neutrality, and drying to obtain alkali fiber;
s2: chemical modification, namely oxidizing the alkali fibers by adopting sodium perchlorate: adding alkali fiber into 12g/L sodium periodate-ethanol (5%) solution (the solid-to-liquid ratio of the alkali fiber to the sodium periodate is 1: 40g/mL), reacting at 45 ℃ in a dark place for 4h, and continuously stirring in the reaction process; after the oxidation reaction, adding a proper amount of glycol into the reaction system to continue the reaction for 30min, and removing the unreacted sodium periodate; filtering the product after the reaction is finished, fully washing and then drying in vacuum to obtain oxidized fiber;
under the protection of nitrogen, placing the oxidized fiber in a pyridine refluxing medium (the solid-to-liquid ratio of the oxidized fiber to the medium is 1: 20g/mL), adding maleic anhydride (the mass ratio of the oxidized cellulose to the maleic anhydride is 1: 6) for reacting for 6h at intervals of 30min for 3 times, filtering the product, washing with acetone, ethanol and deionized water in sequence, and then using saturated NaHCO3Soaking the solution for 30min, filtering, washing to neutrality, and vacuum drying at 50 deg.C to obtain product S; dissolving guanosine in DMF (the mass ratio of the oxidized cellulose to the guanosine is 1: 6), adding EDC and DMAP (the mass ratio of EDC, DMAP and guanosine is 1: 0.2: 1.4), stirring for 15min, adding the product S, and continuously stirring for reacting for 48 h. Pouring the reaction product into water, extracting with ethyl acetate, washing with saturated sodium bicarbonate solution and saturated brine respectively, drying the organic phase with anhydrous sodium sulfate overnight, filtering, separating with silica gel column chromatography (eluent is ethyl acetate and petroleum ether at a volume ratio of 1: 2), distilling under reduced pressure, and vacuum drying to obtain product A;
and (2) putting the product A into a diaminopimelic acid (the mass ratio of oxidized cellulose to diaminopimelic acid is 1: 12) water solution with the concentration of 25g/L, reacting for 2h at the temperature of 60 ℃, and then filtering, washing and drying to obtain the cellulose-based composite adsorbent.
The structural formula after chemical modification is as follows:
Example 2:
consistent with the procedure of example 1, except that: the anhydride in the preparation process is as follows: succinic anhydride; the mass ratio of the oxidized cellulose to the acid anhydride to the guanosine to the diaminopimelic acid is 1: 5: 5.5: 10.
example 3:
consistent with the procedure of example 1, except that: the anhydride in the preparation process is as follows: succinic anhydride; the mass ratio of the oxidized cellulose to the acid anhydride to the guanosine to the diaminopimelic acid is 1: 5.5: 6.5: 11.
example 4:
consistent with the procedure of example 1, except that: and adding sericite powder (the mass ratio of sericite powder to oxidized cellulose is 1: 2) after chemical modification, stirring and mixing uniformly, and drying to obtain the cellulose-based composite adsorbent.
Test example 1:
x-ray photoelectron spectroscopy (XPS) test
Cutting a sample into uniform powder, blank tabletting, attaching the blank tablet on a sample table, carrying out full spectrum scanning and element analysis on the sample within the range of 0-800 eV, and carrying out high-resolution narrow spectrum (C1s) scanning on the sample within the range of 272-296 eV.
The above test was carried out on the sample prepared in example 1, and the results are shown in fig. 1 and 2. FIG. 1 is an XPS spectrum before and after modification of cellulose, scanning shows the appearance of very high intensity photoelectron lines at electron binding energies 287eV, 400eV and 530eV, representing C1s, N1s, O1s, respectively; wherein, the photoelectron characteristic peak of the element N1s appears at the electron binding energy of 400eV in the curve scanned by the modified cellulose, which indicates that the structure contains nitrogen element. After peak separation treatment, as shown in fig. 2, five photoelectron characteristic peaks at electron binding energies of 284.6eV, 285.9eV, 286.5eV, 287.7eV and 288.9eV correspond to C-C, C-N, C-O, C ═ N and C ═ O bonds, respectively; the appearance of characteristic peaks for C-N, C ═ N and C ═ O further confirmed that maleic anhydride, guanosine and diaminopimelic acid were grafted onto cellulose via chemical bonds.
Test example 2:
static adsorption experiment
Respectively dissolving appropriate amount of CR, MB and Pb (NO) in deionized water3)2、CuCl2·2H2O, preparing CR, MB and Pb with the concentration of 1000mg/L2+、Cu2+The solution is ready for use. In which Pb is2+、Cu2+The dosage of the adsorbent in the solution is 1.0g/L, and the dosage of the adsorbent in the CR and MB solutions is 2.0 g/L; the experiments are all carried out in a water bath environment at 30 ℃, and the oscillation is carried out for a certain timeAnd taking the supernatant to test the concentration after adsorption, and calculating the adsorption capacity. Adsorption capacity QeCalculated from the following equation:
Qe＝(C0-Ce)×V/M
wherein, C0And CeRespectively representing the initial concentration and the adsorption equilibrium concentration of the pollutant solution, mg/L; v is the volume of contaminant solution, L; m is the mass of the adsorbent used in the adsorption experiments, g.
The results of the adsorption performance test on the samples obtained in examples 1 to 4 are shown in FIG. 3. Analysis in the figure shows that the samples prepared in examples 1-4 have excellent adsorption capacity on heavy metal ions and dyes, wherein the adsorption capacity on the metal ions is more than 160mg/g, and the adsorption capacity on the dyes is more than 200mg/g, which indicates that the adsorption performance of the bagasse substrate is greatly improved by chemical modification; meanwhile, the saturated adsorption capacity of the sample prepared in example 4 is higher than that of the samples prepared in other examples, which shows that the adsorption performance of the adsorbent can be further improved after the sericite powder is added, and particularly, the adsorption capacity of heavy metal ions and MB is obviously improved.
Determination of the adsorption time at equilibrium
Taking out every 1min, 3min, 5min, 10min, 15min and 20min, standing on a stainless steel filter screen, draining for 5min, weighing and recording in sequence; and then sequentially placing the adsorbed adsorbent in an oven at 80 ℃ for 0.5h, taking out and weighing. The adsorption capacity was calculated by the following formula:
q(g/g)＝(W1-W2-W0)/W0
wherein, W1Mass g after standing for 5min after adsorption by the adsorbent; w2Mass of water adsorbed by the adsorbent, g; w0Is the mass of the adsorbent itself, g.
The above-described tests were carried out on the samples obtained in example 1 and example 4, and the results are shown in FIG. 4. As can be seen from the figure, the adsorption capacity was substantially constant over time, indicating that adsorption equilibrium had been reached. Example 4 takes significantly less time to reach adsorption equilibrium than example 1, indicating that the addition of sericite powder can increase the adsorption rate of the adsorbent.
Cyclic utilization performance
Desorbing the adsorbent adsorbed with heavy metal ions and dye with different desorbing effects, and treating Pb with 0.5mol/L EDTA solution2+、Cu2+Desorbing, and recovering and drying the adsorbent to adsorb the similar metal ions; adsorbing agent loaded with CR, desorbing with 0.1M NaOH aqueous solution and MB with 0.1M HCl solution, shaking at 30 deg.C for 4 hr, recovering dried adsorbent, and adsorbing similar dye again. The adsorption cycle was repeated 5 times, and the change in adsorption capacity of the adsorbent was compared to determine the recycling value.
The above test was performed on the sample prepared in example 1, and the results are shown in fig. 5. As can be seen from the figure, after 5 times of adsorption-desorption, the adsorption capacities for metal ions and dyes are reduced to different degrees; but the adsorption capacity is maintained to be more than 90% of the first adsorption capacity, which shows that the cellulose-based composite adsorbent prepared by the invention has better regenerability, can be used as a regenerable adsorption material, and can reduce the application cost by recycling the adsorbent.
Conventional techniques in the above embodiments are known to those skilled in the art, and therefore, will not be described in detail herein.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (9)
1. A method for preparing a cellulose-based composite adsorbent for wastewater treatment, comprising:
s1: bagasse pretreatment, namely separating, purifying and crushing bagasse raw materials, and then carrying out ultrasonic-alkali liquor-ultrasonic combined pretreatment to generate alkali fibers;
s2: chemically modifying, namely oxidizing the alkali fiber by adopting sodium perchlorate to obtain oxidized fiber;
placing the oxidized fiber in a pyridine or N, N-dimethylacetamide refluxing medium, adding acid anhydride for reaction, washing, dipping, filtering and drying, and then carrying out esterification reaction with guanosine to obtain a product A;
and putting the product A into a diaminopimelic acid aqueous solution for constant-temperature reaction, and then washing and drying to obtain the cellulose-based composite adsorbent.
2. The method for preparing a cellulose-based composite adsorbent for wastewater treatment according to claim 1, wherein: the structural formula of the cellulose-based composite adsorbent in the step S2 is as follows:
3. The preparation method of the cellulose-based composite adsorbent for wastewater treatment according to claim 1, wherein: the mass ratio of the oxidized cellulose to the acid anhydride to the guanosine to the diaminopimelic acid is 1: 5-6: 5.5-6.5: 10 to 12.
4. The method for preparing the cellulose-based composite adsorbent for wastewater treatment according to claim 1, wherein: the oxidation treatment in step S2 is specifically prepared by: the concentration of the sodium periodate aqueous solution is 10-12 g/L, and the solid-to-liquid ratio of the alkali cellulose to the sodium periodate aqueous solution is 1: 40-48 g/mL; the temperature reaction is 40-50 ℃, and the reaction time is 3-4 h; after the reaction is finished, the cellulose base is filtered off, washed to neutrality and dried in vacuum.
5. The method for preparing the cellulose-based composite adsorbent for wastewater treatment according to claim 1, wherein: in the step S2, the acid anhydride is one of succinic anhydride, maleic anhydride and acetic anhydride.
6. The method for preparing the cellulose-based composite adsorbent for wastewater treatment according to claim 1, wherein: in the step S2, the solid-to-liquid ratio of the oxidized fiber to the reaction medium is 1: 20-25 g/mL.
7. The cellulose-based composite adsorbent for wastewater treatment manufactured by the manufacturing method of claim 1.
8. The cellulose-based composite adsorbent for wastewater treatment according to claim 7, characterized in that: the adsorption capacity of the adsorbent to heavy metal ions is more than 160mg/g, and the adsorption capacity to dye is more than 200 mg/g.
9. Use of the cellulose-based composite adsorbent for wastewater treatment according to claim 7 in the field of wastewater treatment.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113786816A (en) * | 2021-09-30 | 2021-12-14 | 长江生态环保集团有限公司 | Preparation method and application of modified natural cellulose adsorbent for repairing cadmium-polluted soil |
| CN117920150A (en) * | 2024-03-22 | 2024-04-26 | 北京大学 | Cellulose porous nanocomposite and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113786816A (en) * | 2021-09-30 | 2021-12-14 | 长江生态环保集团有限公司 | Preparation method and application of modified natural cellulose adsorbent for repairing cadmium-polluted soil |
| CN117920150A (en) * | 2024-03-22 | 2024-04-26 | 北京大学 | Cellulose porous nanocomposite and preparation method and application thereof |
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