CN113559827B - Bacterial cellulose composite aerogel capable of efficiently adsorbing methylene blue and preparation method thereof - Google Patents

Bacterial cellulose composite aerogel capable of efficiently adsorbing methylene blue and preparation method thereof Download PDF

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CN113559827B
CN113559827B CN202110871977.0A CN202110871977A CN113559827B CN 113559827 B CN113559827 B CN 113559827B CN 202110871977 A CN202110871977 A CN 202110871977A CN 113559827 B CN113559827 B CN 113559827B
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bacterial cellulose
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methylene blue
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李湘祁
严卓锋
肖绍峰
夏志强
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Fuzhou University
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    • 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
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
    • B01J20/291—Gel 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
    • 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
    • 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
    • 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
    • C02F2101/38—Organic compounds containing nitrogen
    • 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
    • C02F2101/40—Organic compounds containing sulfur

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Abstract

The invention discloses a bacterial cellulose composite aerogel capable of efficiently adsorbing methylene blue and a preparation method thereof. The bacterial cellulose and the sodium alginate which are adopted by the invention are cheap, renewable and degradable biomass raw materials, the mechanical property of the aerogel is obviously improved after the aluminum chloride hexahydrate crosslinking treatment and the modification of the anionic surfactant, the aerogel can more efficiently adsorb methylene blue, the removal rate of the methylene blue with the concentration of 50mg/l can reach 98.92%, and the original state can be still kept after the methylene blue in the aerogel is removed by an alcohol cleaning mode due to higher mechanical property, so that the recyclable, renewable and degradable biomass aerogel has high practical value and application prospect.

Description

Bacterial cellulose composite aerogel capable of efficiently adsorbing methylene blue and preparation method thereof
Technical Field
The invention belongs to the technical field of adsorption materials, and relates to a bacterial cellulose composite aerogel for efficiently adsorbing methylene blue and a preparation method thereof.
Background
The water body pollution is an important problem which is concerned globally, and Methylene Blue (MB) as a cationic dye (also called basic dye) is the most common substance for dyeing cotton, wood and silk, and has wide application in chemical, biological, medical and printing and dyeing industries. However, methylene blue has certain toxicity, can burn eyes when being contacted with the methylene blue carelessly, is used as a representative pollutant in printing and dyeing wastewater, and is widely applied in industry to cause serious pollution to water environment caused by industrial wastewater containing the methylene blue. Therefore, in the last few years, much attention has been paid to how to effectively remove toxic and harmful MB from wastewater.
The biomass material has wide sources, and mainly comprises rice hulls, fruit peels, wood, plant fibers and the like. Also has the advantages of reproducibility, degradability and the like. There are many studies related to the pretreatment and application of biomass to wastewater pollution. However, the processing method of the biomass material mainly focuses on the processing of the porous carbon material, and patent No. CN 112225212A obtains the porous carbon material with a large number of micropores and mesopores by hydrothermally carbonizing the biomass material, activating the biomass material with potassium citrate, and then acid-washing the biomass material after activation. And most of the carbon materials exist in a powdery form, so that the carbon materials are difficult to recover in practical application and realize secondary utilization. Therefore, how to recover the dye adsorbed by the biomass material and realize recycling of the adsorbent is one of the hot spots of research interest of the biomass dye adsorbent.
The cellulose aerogel has large surface area, high porosity and a physical or chemical crosslinking structure, can quickly absorb water with the mass being hundreds of thousands of times of the self mass, and can keep a certain shape and a three-dimensional space structure in water. Can effectively improve the defect that the powder adsorption material is difficult to recycle. The bacterial cellulose has high tensile strength, has an elastic modulus which is several times to more than ten times higher than that of common plant fibers, and a large number of active groups on the surface, and can be functionalized by modification and crosslinking, thereby becoming a research hotspot.
The method takes the bacterial cellulose with a large number of active groups on the surface and the sodium alginate as raw materials, takes the aluminum chloride hexahydrate with certain sewage purification capacity as a cross-linking agent for the first time, prepares the high-toughness bacterial cellulose composite aerogel, and further improves the adsorption capacity of the high-toughness bacterial cellulose composite aerogel on organic dyes by loading an anionic surfactant. The aerogel overcomes the defect that a large amount of adsorbing materials are difficult to recover, and adsorbed methylene blue can be removed through alcohol, so that the recycling of the aerogel is realized.
Disclosure of Invention
The invention aims to provide a simple, convenient and environment-friendly preparation method of recyclable and easily-recycled three-dimensional cellulose composite aerogel with high adsorption capacity aiming at the defects of the prior art.
In order to realize the purpose, the invention adopts the following technical scheme:
a method for preparing bacterial cellulose composite aerogel capable of being recycled for adsorbing methylene blue dye for multiple times comprises the following steps:
(a) Cleaning the bacterial cellulose membrane, cutting into small pieces, putting the small pieces into a grinder, adding a proper amount of deionized water, grinding into slurry, and fully and uniformly stirring by a homogenizer to obtain the bacterial cellulose dispersion liquid.
(b) Sodium alginate and deionized water in certain proportion are weighed and placed in a beaker, and are stirred continuously at room temperature to be mixed uniformly.
(c) And (c) putting an appropriate amount of the solution prepared in the step (a) and the bacterial cellulose dispersion liquid treated in the step (b) into a beaker, uniformly mixing, and carrying out ultrasonic treatment for 20min. Placing in a freeze drier, pre-freezing at-65 deg.C for 12 hr, and vacuum drying for 48 hr. And obtaining the bacterial cellulose sodium alginate composite aerogel.
(d) And (c) soaking the composite aerogel sample prepared in the step (c) in a solution taking aluminum chloride hexahydrate as a cross-linking agent for a period of time, and then washing with deionized water to obtain the BC-Al-SA aerogel.
(e) And (d) putting the sample prepared in the step (d) in a solution prepared by an anionic surfactant for a period of time, and then washing with deionized water to obtain the cationic dye adsorption type aerogel.
Preferably, the mass fraction of the bacterial cellulose dispersion liquid in the step (a) is 0.64wt%
Preferably, the mass fraction of the sodium alginate solution in the step (b) is 0.64wt%
Preferably, the mass ratio of the bacterial cellulose to the sodium alginate in the step (c) is 1.
Preferably, the crosslinking agent used in the step (d) is aluminum chloride hexahydrate solution with the mass fraction of 1.28 weight percent.
Preferably, the crosslinking time in step (d) is 5h.
Preferably, in the step (e), the anionic surfactant is one of sodium dodecyl benzene sulfonate and a sodium fatty alcohol-polyoxyethylene ether sulfate aqueous solution, and the concentration of the anionic surfactant is 0.5wt%
Preferably, the soaking time in the step (e) is 12h.
The invention has the beneficial effects that:
(1) The invention has the advantages of low requirement on equipment, easy implementation and low preparation cost by simple methods such as mechanical stirring, vacuum freeze drying, surface modification and the like.
(2) The blocky cellulose aerogel with the high specific surface area prepared by the invention overcomes the defect that the traditional biochar adsorbing material and powdery adsorbing material are difficult to recycle.
(3) The cationic dye type aerogel adsorbent with high adsorption rate and high adsorption capacity is obtained, and the removal rate of methylene blue with the concentration of 50mg/l can reach 98.92%.
(4) The aerogel prepared by the invention has good flexibility, after the aerogel is adsorbed, methylene blue in the aerogel can be removed in an alcohol cleaning mode, and when the aerogel is soaked in methylene blue again for adsorption, the aerogel can be adsorbed again, so that the cyclic utilization of the aerogel is realized.
(5) After the aerogel is modified by two anionic surfactants, namely sodium dodecyl benzene sulfonate or fatty alcohol-polyoxyethylene ether sodium sulfate, the adsorption capacity of the composite aerogel on methylene blue is remarkably improved. The preparation method of the methylene blue efficient adsorbent is also suitable for the plant cellulose aerogel adsorbent, and has wide application prospect.
Drawings
FIG. 1 a is a sample plot of the material prepared in example 3: the block-shaped aerogel is placed on the blade with the leaf lines still, the characteristic of low density of the block-shaped aerogel is proved, and b is a color change diagram of the solution before and after the sample absorbs the methylene blue solution: the sample is placed in an oscillator with the rotating speed of 200r/min for adsorption experiment, so that the oscillating aerogel can effectively adsorb methylene blue in the aqueous solution and still can keep the original blocky structure, and the recovery and reuse of the aerogel are guaranteed;
FIG. 2 is a scanning electron micrograph of the material prepared in example 3; (a) Is a scanning electron microscope image of the BC-Al-SA aerogel with magnification of 50X; (b) Is a scanning electron microscope image of BC-Al-SA aerogel with magnification of 2.00 KX; (c) Is a scanning electron microscope image of BC-Al-SA-SDBS aerogel with magnification of 50X; (d) Is a scanning electron microscope image of BC-Al-SA-SDBS aerogel with the magnification of 2.00 KX; from (a) and (c), the aerogel before and after modification is in a porous structure, so that the aerogel has a high specific surface area, and connecting fiber filaments can be observed among holes, which shows that the bacterial cellulose, the sodium alginate and the aluminum chloride hexahydrate have good crosslinking effect, so that the aerogel has high mechanical property; from (b), (d), it can be seen that under the same magnification, the unmodified BC-Al-SA aerogel surface is smooth, no particulate matter is observed, and the modified BC-Al-SA-SDBS aerogel surface is loaded with many fine particles, indicating that the surfactant has been successfully loaded on the composite aerogel surface;
FIG. 3 is a graph of the adsorption profile of the material prepared in example 3; as can be seen from the figure, the composite aerogel modified by the anionic surfactant has better adsorption rate and adsorption capacity than the composite aerogel before the composite aerogel is unmodified;
FIG. 4 is a quasi-first order kinetic adsorption fit curve for the material prepared in example 3: coefficient of correlation R 2 =0.9591；
FIG. 5 is a quasi-second order kinetic adsorption fit curve of the material prepared in example 3, correlation coefficient R 2 =0.99584。
Detailed Description
The invention is further illustrated by the following examples, without restricting its scope to these.
Example 1
The preparation method of the bacterial cellulose composite aerogel capable of being recycled for adsorbing methylene blue dye for multiple times comprises the following steps:
purifying bacterial cellulose purchased in the market, putting the purified bacterial cellulose into a crusher, adding a certain amount of deionized water into the crusher, crushing the mixture to obtain slurry, and uniformly stirring the slurry by a homogenizer to obtain cellulose dispersion liquid.
At room temperature, adding a certain amount of sodium alginate into deionized water to prepare a uniform solution with the mass fraction of 0.64wt%, stirring for 1h, adding 5g of the solution into 5g of bacterial cellulose dispersion liquid with the mass fraction of 0.64wt%, stirring for 5h, and performing ultrasonic treatment for 20min to obtain a uniformly dispersed mixed solution. Pouring the solution into a beaker with the volume of 25ml, placing the beaker in a freeze dryer for pre-freezing for 12 hours, and then carrying out vacuum drying for 48 hours in a vacuum freeze dryer at the temperature of-65 ℃ to finally prepare the sodium alginate/bacterial cellulose composite aerogel. And (2) placing the obtained composite aerogel in an aqueous solution with the mass fraction of 1.28wt% of aluminum chloride hexahydrate for crosslinking for 5 hours, washing the composite aerogel with deionized water for 3-4 times to remove an unreacted crosslinking agent to obtain BC-Al-SA composite aerogel, placing the aerogel in an aqueous solution with the mass fraction of 0.5wt% of lauryl sodium sulfate for soaking for 12 hours to complete surface modification, and then washing the aerogel with deionized water for 3-4 times to remove an unreacted modifying agent. Placing the mixture in a freeze dryer for pre-freezing for 12h, and then carrying out vacuum drying in a vacuum freeze dryer at-65 ℃ for 24h to obtain a sample BC-Al-SA-SLS aerogel.
In the adsorption performance test, 50mg/L methylene blue solution is selected for testing, 20mg of BC-Al-SA-SLS is weighed and added into 20ml of 50mg/L methylene blue solution for stirring in a shaking way, and the removal rate of MB is 80.73 percent after 60min of shaking. Sodium dodecyl sulfate only has one sulfate radical adsorption site with negative charge, and the removal rate of the aerogel on MB cannot be obviously improved.
Example 2
The preparation method of the bacterial cellulose composite aerogel capable of being recycled for adsorbing methylene blue dye for multiple times comprises the following steps:
purifying commercially available bacterial cellulose, putting the purified bacterial cellulose into a crusher, adding a certain amount of deionized water into the crusher, crushing the mixture to obtain slurry, and uniformly stirring the slurry by a homogenizer to obtain cellulose dispersion.
At room temperature, adding a certain amount of sodium alginate into deionized water to prepare a uniform solution with the mass fraction of 0.64wt%, stirring for 1h, adding 5g of the solution into 5g of bacterial cellulose dispersion liquid with the mass fraction of 0.64wt%, stirring for 5h, and performing ultrasonic treatment for 20min to obtain a uniformly dispersed mixed solution. Pouring the solution into a beaker with the volume of 25ml, placing the beaker in a freeze dryer for pre-freezing for 12 hours, and then carrying out vacuum drying for 48 hours in a vacuum freeze dryer at the temperature of-65 ℃ to finally prepare the sodium alginate/bacterial cellulose composite aerogel. Placing the obtained composite aerogel in an aluminum chloride hexahydrate solution with the mass fraction of 1.28wt% for crosslinking for 5 hours, then washing the composite aerogel for 3-4 times by using deionized water to remove unreacted crosslinking agents to obtain BC-Al-SA composite aerogel, then placing the aerogel in an aqueous solution with the mass fraction of 0.5wt% of sodium fatty alcohol polyoxyethylene ether sulfate (AES) for soaking for 12 hours to complete surface modification, and then washing the aerogel for 3-4 times by using deionized water to remove unreacted modifying agents. Placing the mixture in a freeze dryer for pre-freezing for 12h, and then carrying out vacuum drying in a vacuum freeze dryer at-65 ℃ for 24h to obtain a sample BC-Al-SA-AES aerogel.
In the adsorption performance test, 50mg/L methylene blue solution is selected for testing, 20mg of BC-Al-SA-AES is weighed and added into 20ml of 50mg/L methylene blue solution for stirring and shaking, and the removal rate of MB is 97.88% after shaking for 60 min. Compared with sodium dodecyl sulfate, the fatty alcohol-polyoxyethylene ether sodium sulfate has longer hydrophobic carbon chain, and the polyoxyethylene chain increases the polarity of the surfactant, so that the surfactant is easier to perform electrostatic adsorption with MB molecules, and the adsorption amount of the surfactant is higher than that of sodium dodecyl sulfate which is an anionic surfactant.
Example 3
The preparation method of the bacterial cellulose composite aerogel capable of being recycled for adsorbing methylene blue dye for multiple times comprises the following steps:
purifying commercially available bacterial cellulose, putting the purified bacterial cellulose into a crusher, adding a certain amount of deionized water into the crusher, crushing the mixture to obtain slurry, and uniformly stirring the slurry by a homogenizer to obtain cellulose dispersion.
At room temperature, adding a certain amount of sodium alginate into deionized water to prepare a uniform solution with the mass fraction of 0.64wt%, stirring for 1h, adding 5g of the solution into 5g of bacterial cellulose dispersion liquid with the mass fraction of 0.64wt%, stirring for 5h, and performing ultrasonic treatment for 20min to obtain a uniformly dispersed mixed solution. Pouring the solution into a beaker with the volume of 25ml, placing the beaker in a freeze dryer for pre-freezing for 12 hours, and then carrying out vacuum drying for 48 hours in a vacuum freeze dryer at the temperature of-65 ℃ to finally prepare the sodium alginate/bacterial cellulose composite aerogel. Placing the obtained composite aerogel into an aluminum chloride hexahydrate aqueous solution with the mass fraction of 1.28wt% for crosslinking for 5 hours, then washing the composite aerogel with deionized water for 3-4 times to remove unreacted crosslinking agents to obtain BC-Al-SA composite aerogel, then placing the aerogel into an aqueous solution with the mass fraction of 0.5wt% of Sodium Dodecyl Benzene Sulfonate (SDBS) for soaking for 12 hours to complete surface modification, and then washing the composite aerogel with deionized water for 3-4 times to remove unreacted modifying agents. Placing the mixture in a freeze dryer for pre-freezing for 12h, and then carrying out vacuum drying in a vacuum freeze dryer at the temperature of-65 ℃ for 24h to obtain a sample BC-Al-SA-SDBS aerogel.
In the adsorption performance test, 50mg/L methylene blue solution is selected for testing, 20mg of BC-Al-SA-SDBS is weighed and added into 20ml of 50mg/L methylene blue solution for stirring in an oscillating way, and the removal rate of MB is 94.08 percent after 60min of oscillation. Compared with sodium dodecyl sulfate, sodium dodecyl benzene sulfonate has a benzene ring structure with large pi bonds besides containing sulfate radicals, and negative charges exist in the upper part and the lower part of the ring structure to form pi electron polarized adsorption, so that the removal rate of the BC-Al-SA-SDBS aerogel on MB is remarkably improved.
Table 1 shows the adsorption kinetics parameters of example 3 for the dye. The fitting degree of the quasi-second order kinetic equation is higher, so that the adsorption condition of the aerogel can be described through the quasi-second order kinetics.
TABLE 1 kinetic parameters of dye adsorption by BC-Al-SA-SDBS
Figure DEST_PATH_IMAGE001
The above description is only a preferred embodiment of the present invention, and all the equivalent changes and modifications made according to the claims of the present invention should be covered by the present invention.

Claims (5)

1. The bacterial cellulose composite aerogel capable of efficiently adsorbing methylene blue is characterized in that: the preparation method comprises the steps of adopting bacterial cellulose and sodium alginate as carriers and aluminum chloride hexahydrate as a cross-linking agent, obtaining the high-toughness aerogel through freeze drying, and then adding an anionic surfactant as a modifier to obtain the bacterial cellulose composite aerogel capable of efficiently adsorbing methylene blue; the method specifically comprises the following steps:
(1) Cleaning a bacterial cellulose membrane, cutting into small pieces, adding deionized water into a pulverizer, grinding into slurry, and uniformly stirring to obtain a bacterial cellulose dispersion liquid;
(2) Continuously stirring sodium alginate and deionized water at room temperature to uniformly mix;
(3) Uniformly mixing the solution prepared in the step (2) and the bacterial cellulose dispersion liquid prepared in the step (1), carrying out ultrasonic treatment, then carrying out freeze-drying treatment, soaking the aerogel obtained after the freeze-drying treatment in a cross-linking agent solution, and washing with deionized water after the cross-linking treatment to remove the unreacted cross-linking agent, thus obtaining the BC-Al-SA aerogel;
(4) Soaking the aerogel crosslinked in the step (3) in an anionic surfactant solution, washing with deionized water after modification treatment to remove unreacted modifier, and drying to obtain the bacterial cellulose composite aerogel capable of efficiently adsorbing methylene blue;
in the step (3), the mass ratio of the bacterial cellulose to the sodium alginate is 1; the cross-linking agent used in the step (3) is an aluminum chloride hexahydrate solution with the mass fraction of 1.28%, and the time of cross-linking treatment is 5 hours; in the step (4), the anionic surfactant is one of sodium dodecyl benzene sulfonate and fatty alcohol-polyoxyethylene ether sodium sulfate aqueous solution, and the concentration of the anionic surfactant is 0.5wt%.
2. The bacterial cellulose composite aerogel capable of efficiently adsorbing methylene blue according to claim 1, wherein: the mass fraction of the bacterial cellulose dispersion liquid in the step (1) is 0.64%.
3. The bacterial cellulose composite aerogel capable of efficiently adsorbing methylene blue as claimed in claim 1, wherein: the mass fraction of the sodium alginate solution in the step (2) is 0.64%.
4. The bacterial cellulose composite aerogel capable of efficiently adsorbing methylene blue according to claim 1, wherein: in the step (3), the freeze-drying temperature is-65 ℃, and the drying time is 48h.
5. The bacterial cellulose composite aerogel capable of efficiently adsorbing methylene blue according to claim 1, wherein: and (4) soaking the modifier solution in the step (4) for 12 hours.
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