CN112844324A - Lignin/manganese oxide composite adsorption material and preparation method and application thereof - Google Patents

Lignin/manganese oxide composite adsorption material and preparation method and application thereof Download PDF

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CN112844324A
CN112844324A CN201911173398.8A CN201911173398A CN112844324A CN 112844324 A CN112844324 A CN 112844324A CN 201911173398 A CN201911173398 A CN 201911173398A CN 112844324 A CN112844324 A CN 112844324A
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lignin
manganese oxide
kmno
oxide composite
adsorption
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CN112844324B (en
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金明杰
翟睿
陈相雪
许召贤
闻志强
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Nanjing University of Science and Technology
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Nanjing University of Science and Technology
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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
    • 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
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • 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
    • 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
    • C02F2101/308—Dyes; Colorants; Fluorescent agents

Abstract

The invention discloses a lignin/manganese oxide composite adsorption material and a preparation method and application thereof. The method is carried out by reacting lignin with KMnO4Mixing and reacting in the solution, and separating to obtain the lignin/manganese oxide composite material. The lignin/manganese oxide composite material prepared by the invention is prepared by taking cheap lignin as a raw material and potassium permanganate as an oxidant through oxidation-reduction reaction, the preparation method is simple, the preparation process can be completed at room temperature, toxic and harmful chemical reagents are not needed, the preparation cost is low, the efficiency is high, the energy consumption is low, the operation is convenient, and the large-scale production is easy to realize. The lignin/manganese oxide composite material has good treatment effect on dye wastewater, and has the advantages ofThe adsorption rate is fast, the adsorption capacity is large and the removal efficiency is high.

Description

Lignin/manganese oxide composite adsorption material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of adsorption materials, and relates to a lignin/manganese oxide composite adsorption material and a preparation method and application thereof.
Background
The biomass is a renewable energy widely distributed on the earth, mainly comprises cellulose, hemicellulose and lignin, but is mainly used as cheap fuel or randomly discharged, so that resource waste and environmental pollution are caused. Therefore, the development of efficient biomass utilization technology has important significance for reducing environmental pollution and realizing high-value utilization of biomass resources.
The lignin is the main component of the lignocellulose biomass, contains rich functional groups such as hydroxyl, aldehyde group and the like, and has a certain adsorption effect on dye and metal ions. However, unmodified or treated lignin has a low adsorption capacity for contaminants and poor regenerability, limiting further applications of lignin as an adsorbent. In order to improve the adsorption efficiency of lignin on pollutants, the current modification method mainly comprises the following steps: surface modification, carbonization, and compounding. The composite method is used for preparing the composite material by compounding the lignin and the organic/inorganic compound, and can combine the advantages of the lignin and other materials, improve the surface adsorption characteristic and improve the adsorption capacity. Albadarin takes lignin as a substrate, and a lignin/chitosan composite adsorption material is prepared, wherein the maximum adsorption quantity of methylene blue is 36mg/g [ Albadarin Ahmad B., Collins Maurice N., Nausad Mu, Shirazian sweet, Walker Gavin, Mangwandi C., activated lignin-chitosan extended blends for influencing adsorption of methyl blue. ChemEng J,2017,307: 264-. However, the adsorption capacity of the lignin/chitosan composite adsorption on organic pollutants is still low, and the application of the lignin/chitosan composite adsorption in the field of wastewater treatment is limited.
The manganese oxide has a good effect of removing organic matters, metal ions and the like in water. The artificially synthesized manganese oxide compound and the natural manganese ore taking the manganese oxide as the main component have good adsorption effects on motherland, organic pesticides and dyes in water. However, the preparation process of the manganese oxide with good adsorption performance is complex, and most of the manganese oxide relates to the use of toxic and harmful chemical reagents and reaction conditions of high temperature and high pressure, so that the manganese oxide has high cost and great environmental hazard, and the application of the manganese oxide in the field of wastewater treatment is limited.
Disclosure of Invention
The invention provides a lignin/manganese oxide composite adsorption material and a preparation method and application thereof. According to the method, cheap lignin is used as a source, potassium permanganate is used as an oxidant, and manganese oxide is generated through an oxidation-reduction reaction between the potassium permanganate and the lignin, so that the effect of modifying the surface of the lignin is realized, and the adsorption effect of the lignin on pollutants is greatly improved.
The technical scheme of the invention is as follows:
the preparation method of the lignin/manganese oxide composite adsorption material comprises the following steps: mixing lignin with KMnO4And mixing the solutions for reaction, and separating to obtain the lignin/manganese oxide composite material.
The lignin is derived from lignocellulose biomass such as wheat straw, corn straw, agricultural and forestry waste, rice straw, sorghum straw, soybean straw, forestry waste, wood pulp fiber, wood chips, softwood, hardwood and the like.
The lignin according to the present invention may be untreated biomass or isolated lignin.
The lignin according to the present invention may be a single kind of lignin or a mixture of different kinds of lignin extracted from biomass.
The lignin can be nano-scale lignin particles, micro-scale lignin particles, lignin residues or slurry produced in the paper making process of paper pulp, solid residues rich in lignin obtained after lignocellulose hydrolysis, solid residues containing lignin obtained after lignocellulose pretreatment and the like.
The lignin can be obtained by solvent extraction, mechanical treatment, chemical treatment, enzymatic treatment or microbial treatment.
The lignin according to the present invention may be a lignin solid or a lignin suspension.
The solvent in the lignin suspension of the present invention may be water or a mixture of water and other solvents.
In the present invention, KMnO4The mass ratio of the lignin to the lignin is 1: 100-100: 100, preferably 2: 100-15: 100.
In the present invention, KMnO4The concentration of the solution is 0.1-5 g/L.
In the present invention, KMnO4The reaction time of the lignin and the mixture is 5 min-24 h.
In the present invention, KMnO4The temperature for mixing and reacting with lignin is 4-50 ℃.
In the present invention, KMnO4And mixing the lignin with the lignin for reaction, wherein the pH value is 2-10.
The invention also provides the lignin/manganese oxide composite adsorbing material prepared by the preparation method.
Further, the invention provides an application of the lignin/manganese oxide composite adsorption material in adsorption of organic pollutants.
The organic pollutants can be methylene blue, active black, crystal violet, active blue, methyl orange, rhodamine B and the like.
Compared with the prior art, the invention has the following advantages:
the lignin/manganese oxide composite adsorption material has a good adsorption effect on methylene blue dye, has the characteristics of high adsorption rate, large adsorption capacity and high removal efficiency, has an adsorption capacity of 1250mg/g for 500mg/L methylene blue solution, and is convenient for large-scale production and application.
Drawings
Fig. 1 is a graph showing the effect of adsorption of methylene blue by the lignin/manganese oxide composite in example 1 and example 2.
FIG. 2 shows the amounts of KMnO added in different amounts in example 34And (3) obtaining an adsorption effect diagram of the lignin/manganese oxide composite material on methylene blue after treatment.
FIG. 3 is a scanning electron micrograph of lignin/manganese oxide in example 4.
FIG. 4 is a transmission electron micrograph of lignin/manganese oxide of example 4.
FIG. 5 is an X-ray diffraction pattern of lignin and lignin/manganese oxides from example 4.
FIG. 6 is an infrared spectrum of lignin and lignin/manganese oxides from example 4.
FIG. 7 is a graph showing the effect of adsorption of methylene blue by lignin/manganese oxide in example 4.
Detailed Description
The present invention will be described in more detail with reference to the following examples and the accompanying drawings.
Example 1
Step 1, preparing a lignin suspension: carrying out catalytic hydrolysis on corn straws pretreated by alkali by using cellulase to obtain enzymatic hydrolysis lignin, and dispersing 40mg of enzymatic hydrolysis lignin in 40mL of water to obtain a lignin suspension.
Step 2, KMnO4Preparation of the solution: 50mg of KMnO4Dissolving in 50mL water, mixing well, and preparing to obtain KMnO4And (3) solution.
Step 3, adding 1mLKMno4The solution is slowly dropped into 10mL of lignin suspension to react for 10h, and the lignin/manganese oxide composite material is prepared.
Example 2
Step 1, preparing a lignin suspension: and (3) carrying out catalytic hydrolysis on the corn straws pretreated by the acid by using cellulase to obtain enzymatic hydrolysis lignin, and dispersing 40mg of enzymatic hydrolysis lignin in 40mL of water to obtain a lignin suspension.
Step 2, KMnO4Preparation of the solution: 50mg of KMnO4Dissolving in 50mL water, mixing well, and preparing to obtain KMnO4And (3) solution.
Step 3, mixing 1mL of KMnO4The solution (1mg/mL) was slowly dropped into 10mL of the lignin suspension, and reacted for 10 hours to prepare a lignin/manganese oxide composite material.
Example 3
Step 1, preparing a lignin suspension: carrying out catalytic hydrolysis on corn straws pretreated by alkali by using cellulase to obtain enzymatic hydrolysis lignin, and dispersing 40mg of enzymatic hydrolysis lignin in 40mL of water to obtain a lignin suspension.
Step 2, KMnO4Preparation of the solution: 50mg of KMnO4Dissolving in 50mL water, mixing, and making into final productObtaining KMnO4And (3) solution.
Step 3, mixing 0.2mL, 0.5mL, 1mL, 1.5mL KMnO4The solution was slowly dropped into 10mL lignin suspension, corresponding to KMnO4And the mass ratio of the lignin to the lignin is 2:100, 5:100, 10:100 and 15:100 respectively, and the reaction is carried out for 10 hours to prepare the lignin/manganese oxide composite material.
Example 4
Step 1, preparing a lignin nanoparticle suspension: and (3) carrying out catalytic hydrolysis on the corn straws subjected to the ammonia blasting pretreatment by using cellulase to obtain enzymatic hydrolysis lignin. 40mg of enzymatic lignin was dissolved in 20mL of dimethyl sulfoxide solution to fully dissolve the lignin. And dialyzing the lignin solution in an aqueous solution by using a dialysis bag with the aperture of 3Kda to remove dimethyl sulfoxide to prepare the lignin nanoparticle suspension.
Step 2, KMnO4Preparation of the solution: 50mg of KMnO4Dissolving in 50mL water, mixing well, and preparing to obtain KMnO4And (3) solution.
Step 3, mixing 1mL of KMnO4And slowly dripping the solution into 10mL of lignin nanoparticle suspension, and reacting for 10h to prepare the lignin/manganese oxide composite nano material.
Application example
And (3) freeze-drying the samples prepared in the embodiments, carrying out an adsorption experiment for 4 hours at the conditions of pH 7 and temperature of 25 ℃ by taking methylene blue as a representative pollutant, centrifuging the mixture after the experiment is finished, measuring the absorbance of the supernatant by using a spectrophotometry, determining the concentration of the methylene blue, and calculating the final adsorption amount.
Fig. 1 is a graph showing the effect of adsorption of methylene blue by the lignin/manganese oxide composite materials prepared in examples 1 and 2. As can be seen from the figure, in the methylene blue solution with the initial concentration of 140mg/L, the adsorption amounts of untreated alkali pretreatment enzymatic hydrolysis lignin (alkali lignin) and acid pretreatment enzymatic hydrolysis lignin (acid lignin) to the methylene blue are 63 and 49mg/g respectively, and the adsorption amounts of the alkali lignin/manganese oxide and the acid lignin/manganese oxide are 152 and 129mg/g respectively, which shows that the adsorption capacity of lignin to the methylene blue is greatly improved by compounding with the manganese oxide.
FIG. 2 shows the KMnO added in different amounts in example 34And (3) obtaining an adsorption effect diagram of the lignin/manganese oxide composite material on methylene blue after treatment. It can be seen from the figure that with KMnO4The adsorption amount of the lignin/manganese oxide composite material to methylene blue is gradually increased with the increase of the addition amount, and the KMnO is low4The addition amount can realize the great increase of the adsorption capacity.
FIG. 3 is a scanning electron micrograph of lignin/manganese oxide in example 4. As can be seen from an electron microscope image, the particle size of the lignin/manganese oxide composite particles is within 100nm, and the nanoparticles are aggregated to form a porous structure, so that the specific surface area of the composite material is increased.
FIG. 4 is a transmission electron micrograph of lignin/manganese oxide of example 4. As can be seen from the figure, the lignin is interspersed with manganese oxide particles of about 3-5 nm in size.
FIG. 5 is an X-ray diffraction pattern of lignin and lignin/manganese oxides from example 4. In the X-ray diffraction pattern, the unmodified lignin showed a broad peak near 20 °, indicating the amorphous structure of the lignin, while the spike at 26.8 ° was due to the presence of crystalline impurities in the extracted lignin. Compared with the diffraction pattern of lignin, the lignin/manganese oxide shows crystallization peaks at 10.8 degrees (111) and 36.5 degrees (200), and shows that the formed manganese oxide is MnO2(KMnO2,JCPDS No.44-1025).。
FIG. 6 is an infrared spectrum of lignin and lignin/manganese oxide composite particles of example 4. 3263cm in the figure-1The vicinity of the absorption band shows that the wide absorption band is hydrogen bond OH stretching vibration, and is 2912cm-1Nearby adsorption peaks were CH stretching oscillations in methyl, methylene and acetylene groups at 2358cm-1The absorption peak at 1583cm due to C ═ O vibration in the keto group-1,1512cm-1,1461cm-1The peak at (a) is due to aromatic skeleton vibration in the lignin. 1234cm-1The peak value of absorption is syringyl ring and C ═ O stretching vibration, and is 1066cm-1The absorption peak at (A) is due to the secondary and primary alcoholsOr C-O in aliphatic ethers. By comparison, 1234cm was present in the lignin/manganese oxide composite particles-1And 1066cm-1The peak intensity is significantly reduced. This indicates that the manganese oxide formation is predominantly aliphatic ether with KMnO4As a result of redox reactions.
FIG. 7 is a graph showing the effect of adsorption of methylene blue by lignin/manganese oxide in example 4. As shown in the figure, in 500mg/L methylene blue solution, the removal efficiency of the methylene blue is greatly improved along with the increase of the dosage of the adsorbent, and the adsorption quantity is gradually reduced. When the dosage of the adsorbent is 0.8g/L, the removal rate of the methylene blue is 95 percent; when the dosage of the adsorbent is 0.08g/L, the adsorption quantity is 1250 mg/g. The adsorption capacity of the composite material gradually decreases with increasing adsorbent usage, mainly because the adsorption sites on the surface of the composite material are not saturated in the presence of higher adsorbents. By integrating the influence of the addition amount of the adsorbent on the adsorption efficiency and the adsorption amount, the higher methylene blue removal efficiency and the higher adsorption amount can be realized under the adsorbent dosage of 0.3 g/L.

Claims (10)

1. The preparation method of the lignin/manganese oxide composite adsorption material is characterized by comprising the following steps: mixing lignin with KMnO4And mixing the solutions for reaction, and separating to obtain the lignin/manganese oxide composite material.
2. The method of claim 1, wherein the lignin is derived from lignocellulosic biomass selected from the group consisting of wheat straw, corn stover, agricultural and forestry waste, rice straw, sorghum straw, soybean stover, forestry waste, wood pulp fiber, wood chips, softwood and hardwood; the lignin is single kind lignin or mixture of different kinds of lignin extracted from biomass.
3. The method of claim 1, wherein the lignin is an untreated biomass or an isolated lignin.
4. The method according to claim 1, wherein the lignin is selected from the group consisting of nano-sized lignin particles, micro-sized lignin particles, lignin residues or pulp from pulp and paper making processes, lignin-rich solid residues obtained from lignocellulosic hydrolysis, and lignin-containing solid residues obtained from lignocellulosic pretreatment, and the lignin is obtained by solvent extraction, mechanical treatment, chemical treatment, enzymatic treatment, and microbial treatment.
5. The method of claim 1, wherein the lignin is a lignin solid or a lignin suspension; the solvent in the lignin suspension is water or a mixed solution of water and other solvents.
6. The method of claim 1, wherein KMnO is used as a carrier4The mass ratio of the lignin to the lignin is 1: 100-100: 100, preferably 2: 100-15: 100.
7. The method of claim 1, wherein KMnO is used as a carrier4The concentration of the solution is 0.1-5 g/L, and KMnO4The reaction time of the lignin and KMnO is 5 min-24 h4The temperature of the mixing reaction of the lignin and the lignin is 4-50 ℃, and the KMnO4And mixing the lignin with the lignin for reaction, wherein the pH value is 2-10.
8. The lignin/manganese oxide composite adsorbing material prepared by the preparation method according to any one of claims 1 to 7.
9. Use of the lignin/manganese oxide composite adsorbent material according to claim 8 for adsorbing organic pollutants.
10. The use according to claim 9, wherein the organic contaminant is methylene blue, reactive black, crystal violet, reactive blue, methyl orange or rhodamine B.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107164433A (en) * 2017-07-12 2017-09-15 天津科技大学 A kind of method of ultrasonic assistant alkalinity potassium permanganate preprocessing lignocellulose
KR20190004035A (en) * 2017-07-03 2019-01-11 대한민국(산림청 국립산림과학원장) MnO2 deposited on lignin based carbon nanofiber mats for symmetric pseudocapacitors
CN109289782A (en) * 2018-10-10 2019-02-01 太原工业学院 A kind of manganese dioxide/corn stover nano material and its preparation method and application
CN109913507A (en) * 2019-03-19 2019-06-21 南京理工大学 Synchronize the lignocellulosic method for refining for carrying out pretreatment and enzyme hydrolysis
CN109971806A (en) * 2017-12-28 2019-07-05 南京理工大学 Mix lignocellulose pretreatment method and its zymotechnique

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20190004035A (en) * 2017-07-03 2019-01-11 대한민국(산림청 국립산림과학원장) MnO2 deposited on lignin based carbon nanofiber mats for symmetric pseudocapacitors
CN107164433A (en) * 2017-07-12 2017-09-15 天津科技大学 A kind of method of ultrasonic assistant alkalinity potassium permanganate preprocessing lignocellulose
CN109971806A (en) * 2017-12-28 2019-07-05 南京理工大学 Mix lignocellulose pretreatment method and its zymotechnique
CN109289782A (en) * 2018-10-10 2019-02-01 太原工业学院 A kind of manganese dioxide/corn stover nano material and its preparation method and application
CN109913507A (en) * 2019-03-19 2019-06-21 南京理工大学 Synchronize the lignocellulosic method for refining for carrying out pretreatment and enzyme hydrolysis

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