CN112121771A - Biomass adsorbent for removing refractory organic pollutants, preparation method and application method thereof - Google Patents
Biomass adsorbent for removing refractory organic pollutants, preparation method and application method thereof Download PDFInfo
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 59
- 239000002028 Biomass Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000002957 persistent organic pollutant Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 31
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 18
- 240000008042 Zea mays Species 0.000 claims abstract description 17
- 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
- GSDSWSVVBLHKDQ-JTQLQIEISA-N Levofloxacin Chemical compound C([C@@H](N1C2=C(C(C(C(O)=O)=C1)=O)C=C1F)C)OC2=C1N1CCN(C)CC1 GSDSWSVVBLHKDQ-JTQLQIEISA-N 0.000 claims abstract description 8
- XMEVHPAGJVLHIG-FMZCEJRJSA-N chembl454950 Chemical compound [Cl-].C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H]([NH+](C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O XMEVHPAGJVLHIG-FMZCEJRJSA-N 0.000 claims abstract description 8
- 229960003376 levofloxacin Drugs 0.000 claims abstract description 8
- 229960004989 tetracycline hydrochloride Drugs 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 25
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 8
- 239000006228 supernatant Substances 0.000 claims description 8
- 241000196324 Embryophyta Species 0.000 claims description 6
- -1 zirconium ions Chemical class 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 11
- 239000003814 drug Substances 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 9
- 239000002154 agricultural waste Substances 0.000 abstract description 8
- 229940079593 drug Drugs 0.000 abstract description 6
- 230000020477 pH reduction Effects 0.000 abstract description 6
- 238000011068 loading method Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 7
- 239000002351 wastewater Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 229920002678 cellulose Polymers 0.000 description 4
- 239000001913 cellulose Substances 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 239000003242 anti bacterial agent Substances 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 229940124350 antibacterial drug Drugs 0.000 description 3
- 229940088710 antibiotic agent Drugs 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 241000282414 Homo sapiens Species 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010170 biological method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- 206010067484 Adverse reaction Diseases 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000006838 adverse reaction Effects 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- GBNDTYKAOXLLID-UHFFFAOYSA-N zirconium(4+) ion Chemical compound [Zr+4] GBNDTYKAOXLLID-UHFFFAOYSA-N 0.000 description 1
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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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0211—Compounds of Ti, Zr, Hf
-
- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0248—Compounds of B, Al, Ga, In, Tl
-
- 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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/485—Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
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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
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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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
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- Chemical & Material Sciences (AREA)
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- Life Sciences & Earth Sciences (AREA)
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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a biomass adsorbent for removing refractory organic pollutants, a preparation method and a use method thereof, belonging to the field of sewage treatment in environmental protection. The invention provides a preparation method of a biomass adsorbent for removing refractory organic pollutants, which takes agricultural waste corn bracts as a raw material, and carries out metal ion loading after acidizing corn bract powder. The invention takes agricultural wastes as raw materials, and prepares the modified biomass material adsorbent by utilizing corn bracts through acidification or alkalization and metal ion loading; the adsorbent can adsorb organic pollutants which are difficult to degrade in water, such as levofloxacin, tetracycline hydrochloride and the like, so that the aim of controlling drug pollution is fulfilled; the invention has the characteristics of waste recycling, wide raw material source, simple and convenient preparation, strong adsorption capacity of the adsorbent and the like.
Description
Technical Field
The invention relates to a biomass adsorbent for removing refractory organic pollutants, a preparation method and a use method thereof, belonging to the field of sewage treatment in environmental protection.
Background
Levofloxacin and tetracycline hydrochloride are widely used antibiotics and have the characteristics of wide antibacterial spectrum, strong antibacterial activity, good curative effect, few adverse reactions and the like. However, due to abuse of antibacterial drugs and unreasonable treatment of wastewater, accumulation of the antibacterial drugs in a water body environment is caused, and the characteristic of difficult biodegradation not only influences normal growth and metabolism of microorganisms and has certain harm to aquatic organisms and human beings, but also can cause drug resistance of germs and generate great threat to ecological systems and human health. Therefore, the development of antibacterial treatment technology in water has important significance and urgent need for environmental protection and the relief of the accumulation of antibiotics in the water environment.
At present, the common method for removing the antibacterial drugs in the water body mainly comprises the following steps: biological, chemical, and physical-chemical methods. The biological method can greatly reduce COD and improve biodegradability. However, the components of the wastewater containing the medicine are complex, and the wastewater containing the medicine contains a large amount of substances which are difficult to degrade and substances with biological toxicity, so that the wastewater treated by a biological method cannot meet the industrial standard. The Fenton oxidation method in the chemical method is a traditional water treatment method which is easy to treat and simple to operate. However, the Fenton oxidation method is applicable to a narrow pH range, generates a large amount of iron mud, has high reagent cost and is easy to corrode a device. The photocatalytic oxidation treatment of pollutants has the characteristics of easy operation control, capability of utilizing solar energy for catalytic degradation, strong oxidizing capability, no secondary pollution and the like. However, the method has the problems of low photocatalytic quantum efficiency, low solar energy utilization rate, difficult recovery of the powdery photocatalyst and the like.
The adsorption method is to utilize porous solid or floc to adsorb the medicine in waste water to the surface or inside micropores so as to separate pollutant from environment effectively. The adsorption method has the advantages of simple operation, no generation of high-toxicity metabolites, wide source of the adsorbent, recoverability and the like, but the adsorbent has the problems of low removal rate or high cost. Therefore, how to improve the removal rate of the adsorbent and find an economically available adsorbent is the key for removing the medicine in the wastewater by using the adsorbent.
Disclosure of Invention
1. Problems to be solved
Aiming at the problem of poor adsorption effect of the adsorbent in the prior art, the invention provides the preparation method of the biomass adsorbent for removing the refractory organic pollutants, which takes the corn bracts which are agricultural wastes as raw materials, and increases the pore area and the active adsorption sites of the adsorbent by carrying out metal ion loading after the acidification treatment of the corn bract powder, so that the adsorption capacity is increased, and the problem of poor adsorption effect of the adsorbent is solved.
Furthermore, the invention also provides a biomass adsorbent prepared by the method for removing the organic pollutants difficult to degrade, and an adsorbent prepared by acidized corn bracts, and the adsorption effect is obvious.
Further, the invention provides a method for adsorbing levofloxacin or tetracycline hydrochloride by using the adsorbent, which not only solves the problem of treatment and disposal of agricultural wastes, realizes secondary utilization, but also reduces drug pollution in water.
2. Technical scheme
In order to solve the problems, the technical scheme adopted by the invention is as follows:
the invention provides a preparation method of a biomass adsorbent for removing refractory organic pollutants, which comprises the following steps,
s100, cleaning and drying plant leaves, and crushing and sieving to obtain powder to be treated; the plant leaves are corn bracts;
s200, mixing the powder to be treated according to the weight ratio of 1 g: adding 0.1mol/L sulfuric acid solution into 25ml of the mixture, and stirring the mixture to react for 24 hours to obtain acidified powder;
s300, taking the acidified powder out, washing the acidified powder to obtain supernatant, wherein the pH value of the supernatant is 6-8, and drying to obtain powder to be loaded;
s400, mixing the powder to be loaded according to the weight ratio of 1 g: 20ml of the solution is put into the metal ion solution, stirred and reacted for 4 hours, and kept stand for 20 hours to obtain a mixed solution;
s500, dropwise and slowly adding a sodium hydroxide solution into the mixed solution until the pH value is 5-7, stirring for reaction for 1 hour, and standing for 24 hours to obtain a load product;
s600, filtering the load product, and drying to obtain the biomass adsorbent.
Preferably, the drying temperature in S100 is 60 ℃.
Preferably, the stirring rate of the stirring reaction in S200 is 180 r/min.
Preferably, the concentration of the metal ion solution in S400 is 0.1-1.5 mol/L.
Preferably, the metal ions contained in the metal ion solution in S400 are one or both of zirconium ions and aluminum ions.
Preferably, the reaction temperature of the stirring reaction in S400 is 30 ℃ and the stirring rate is 180 r/min.
Preferably, the stirring reaction in S500 has a reaction temperature of 30 ℃ and a stirring rate of 120 r/min.
Preferably, the drying temperature in S600 is 40 ℃.
The invention also provides the biomass adsorbent prepared by the preparation method of the biomass adsorbent for removing the refractory organic pollutants.
The invention also provides application of the biomass adsorbent in removing refractory organic pollutants, wherein the refractory organic pollutants are antibiotics such as levofloxacin or tetracycline hydrochloride.
3. Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the preparation method of the biomass adsorbent for removing the organic pollutants difficult to degrade, disclosed by the invention, the agricultural waste corn bracts are used as the raw materials, the raw materials for preparing the adsorbent are easy to obtain, and the reutilization of the wastes is realized; the corn bract powder is subjected to acidification treatment and then metal ion loading, so that the preparation process of the adsorbent is simple and the operation cost is low; the acidification treatment increases the pore area and active adsorption sites of the adsorbent, increases the adsorption capacity and solves the problem of poor adsorption effect of the adsorbent.
(2) According to the preparation method of the biomass adsorbent for removing the refractory organic pollutants, the drying temperature is 40 ℃ or 60 ℃, the reaction temperature is 30 ℃, the treatment process conditions are mild, and the preparation method is suitable for popularization and application.
(3) According to the biomass adsorbent for removing the organic pollutants difficult to degrade, agricultural wastes are used as raw materials, the corn bracts are acidified or alkalized and loaded with metal ions to prepare the modified biomass material adsorbent, so that the modified biomass material adsorbent can adsorb various medicines in a water body, and is low in cost, economic, environment-friendly and wide in application range; the adsorbent can adsorb levofloxacin and tetracycline hydrochloride, thereby achieving the purpose of controlling drug pollution; the invention has the characteristics of waste recycling, wide raw material source, simple and convenient preparation, strong adsorption capacity of the adsorbent and the like.
Detailed Description
The invention is described in detail below with reference to specific exemplary embodiments. It will, however, be understood that various modifications and changes may be made without departing from the scope of the invention as defined in the appended claims. The detailed description is to be construed as illustrative only and not restrictive, and any such modifications and variations are intended to be included within the scope of the invention as described herein. Furthermore, the background is intended to be illustrative of the state of the art as developed and the meaning of the present technology and is not intended to limit the scope of the invention or the application and field of application of the invention.
Example 1
The preparation method of the biomass adsorbent for removing the refractory organic pollutants comprises the following specific steps,
s100, cleaning and drying plant leaves, and crushing and sieving to obtain powder to be treated; the plant leaves are corn bracts; the drying temperature is 60 ℃;
s200, mixing the powder to be treated according to the weight ratio of 1 g: adding 0.1mol/L sulfuric acid solution into 25ml of the mixture, and stirring the mixture for reaction for 24 hours at the stirring speed of 180r/min to obtain acidified powder;
s300, taking the acidified powder out, washing the acidified powder to obtain supernatant, wherein the pH value of the supernatant is 6-8, and drying to obtain powder to be loaded;
s400, mixing the powder to be loaded according to the weight ratio of 1 g: putting 20ml of the mixture into a metal ion solution, stirring the mixture for reaction for 4 hours at the reaction temperature of 30 ℃ and the stirring speed of 180r/min, and standing the mixture for 20 hours to obtain a mixed solution; further, the concentration of the metal ion solution is 0.1-1.5 mol/L, and the metal ions in the metal ion solution are one or two of zirconium ions and aluminum ions;
s500, dropwise and slowly adding a sodium hydroxide solution into the mixed solution until the pH value is 5-7, the reaction temperature is 30 ℃, the stirring speed is 120r/min, stirring and reacting for 1h, and standing for 24h to obtain a load product;
s600, filtering the load product, and drying at 40 ℃ to obtain the biomass adsorbent.
The invention adopts an acid treatment mode, destroys the structure of corn bract, reduces the polymerization degree and the crystallinity of cellulose, can form a swelling porous structure, increases the pore area and the active adsorption sites of the adsorbent, and increases the adsorption capacity. It is worth to say that the method adopts sulfuric acid for acidification treatment, which is more beneficial to hydrolysis of cellulose and hemicellulose, breaks the structure of corn bract, reduces the polymerization degree and the crystallinity of the cellulose, can enable the cellulose to form a swelling porous structure, increases the pore area and active adsorption sites of the adsorbent, and obviously increases the adsorption capacity.
The invention also provides a biomass adsorbent prepared by the method, and an adsorbent prepared from acidified corn bracts, and the adsorption effect is obvious. The modified biomass material adsorbent is prepared by taking agricultural wastes as raw materials and utilizing corn bracts through acidification or alkalization and loading of metal ions, can adsorb various medicines in a water body, and has the advantages of low cost, economy, environmental protection and wide application range. The biomass adsorbent provided by the invention is used for removing organic pollutants in water, such as levofloxacin or tetracycline hydrochloride, so that the problem of treatment and disposal of agricultural wastes is solved, secondary utilization is realized, and drug pollution in water is reduced.
In this example, the specific preparation steps were as follows,
s100, cleaning corn bracts, drying at 60 ℃, crushing, and sieving with a 80-mesh sieve to obtain powder to be treated;
s200, mixing the powder to be treated according to the weight ratio of 1 g: adding 0.1mol/L sulfuric acid solution into 25ml of the mixture, and stirring the mixture for reaction for 24 hours at the stirring speed of 180r/min to obtain acidified powder;
s300, taking the acidified powder out, washing the acidified powder to obtain supernatant, wherein the pH value of the supernatant is 6-8, and drying to obtain powder to be loaded;
s400, mixing the powder to be loaded according to the weight ratio of 1 g: adding 0.5mol/L zirconium ion solution into 20ml of the solution, stirring the solution at the reaction temperature of 30 ℃ and the stirring speed of 180r/min for 4 hours, and standing the solution for 20 hours to obtain a mixed solution;
s500, dropwise and slowly adding a sodium hydroxide solution into the mixed solution until the pH value is 6, wherein the reaction temperature is 30 ℃, the stirring speed is 120r/min, stirring for reacting for 1h, and standing for 24h to obtain a load product;
s600, filtering the load product, and drying at 40 ℃ to obtain the biomass adsorbent.
0.1g of the biomass adsorbent is put into 50ml of levofloxacin solution with 100mg/L, pH being 3, and the adsorption amount can reach 35mg/g after 24 hours of adsorption reaction at the temperature of 30 ℃. 0.1g of the biomass adsorbent is put into 50ml of tetracycline hydrochloride solution with the concentration of 200mg/L, pH being 7, and the adsorption capacity can reach 100mg/g after 24 hours of adsorption reaction at the temperature of 30 ℃.
More specifically, although exemplary embodiments of the invention have been described herein, the invention is not limited to these embodiments, but includes any and all embodiments modified, omitted, combined, e.g., between various embodiments, adapted and/or substituted, as would be recognized by those skilled in the art from the foregoing detailed description. The limitations in the claims are to be interpreted broadly based the language employed in the claims and not limited to examples described in the foregoing detailed description or during the prosecution of the application, which examples are to be construed as non-exclusive. Any steps recited in any method or process claims may be executed in any order and are not limited to the order presented in the claims. The scope of the invention should, therefore, be determined only by the appended claims and their legal equivalents, rather than by the descriptions and examples given above.
Claims (10)
1. A preparation method of a biomass adsorbent for removing refractory organic pollutants is characterized by comprising the following steps: the preparation method comprises the following specific steps of,
s100, cleaning and drying plant leaves, and crushing and sieving to obtain powder to be treated; the plant leaves are corn bracts;
s200, mixing the powder to be treated according to the weight ratio of 1 g: adding 0.1mol/L sulfuric acid solution into 25ml of the mixture, and stirring the mixture to react for 24 hours to obtain acidified powder;
s300, taking the acidified powder out, washing the acidified powder to obtain supernatant, wherein the pH value of the supernatant is 6-8, and drying to obtain powder to be loaded;
s400, mixing the powder to be loaded according to the weight ratio of 1 g: 20ml of the solution is put into the metal ion solution, stirred and reacted for 4 hours, and kept stand for 20 hours to obtain a mixed solution;
s500, dropwise and slowly adding a sodium hydroxide solution into the mixed solution until the pH value is 5-7, stirring for reaction for 1 hour, and standing for 24 hours to obtain a load product;
s600, filtering the load product, and drying to obtain the biomass adsorbent.
2. The preparation method of the biomass adsorbent for removing the refractory organic pollutants as claimed in claim 1, wherein the preparation method comprises the following steps: the drying temperature in S100 is 60 ℃.
3. The preparation method of the biomass adsorbent for removing the refractory organic pollutants as claimed in claim 1, wherein the preparation method comprises the following steps: the stirring rate of the stirring reaction in S200 is 180 r/min.
4. The preparation method of the biomass adsorbent for removing the refractory organic pollutants as claimed in claim 1, wherein the preparation method comprises the following steps: the concentration of the metal ion solution in S400 is 0.1-1.5 mol/L.
5. The preparation method of the biomass adsorbent for removing the refractory organic pollutants as claimed in claim 1, wherein the preparation method comprises the following steps: the metal ions contained in the metal ion solution in S400 are one or both of zirconium ions and aluminum ions.
6. The preparation method of the biomass adsorbent for removing the refractory organic pollutants as claimed in claim 1, wherein the preparation method comprises the following steps: the reaction temperature of the stirring reaction in S400 was 30 ℃ and the stirring rate was 180 r/min.
7. The preparation method of the biomass adsorbent for removing the refractory organic pollutants as claimed in claim 1, wherein the preparation method comprises the following steps: the reaction temperature of the stirring reaction in S500 was 30 ℃ and the stirring rate was 120 r/min.
8. The preparation method of the biomass adsorbent for removing the refractory organic pollutants as claimed in claim 1, wherein the preparation method comprises the following steps: the drying temperature in S600 is 40 ℃.
9. The biomass adsorbent prepared by the preparation method of the biomass adsorbent for removing the refractory organic pollutants in any one of claims 1 to 8.
10. Use of the biomass adsorbent of any one of claim 9 for removing refractory organic pollutants, said refractory organic pollutants being levofloxacin or tetracycline hydrochloride.
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