CN114797788B - A kind of modified chitosan airgel and its preparation method and application - Google Patents
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Abstract
一种改性壳聚糖气凝胶及其制备方法和应用，称取LaCl3•7H2O，ZrOCl2•8H2O，溶于去离子水中，在水浴下搅拌，并滴加NaOH溶液，继续搅拌；然后60℃恒温陈化，分别用去离子水和乙醇洗涤三次，记为溶液A；称取膨润土原料溶于去离子水中，60℃恒温条件下，将溶液A滴入膨润土矿浆中，不断搅拌，完成滴加后继续搅拌，然后在恒温条件下陈化，陈化后的柱撑产物采用离心分离，用去离子水和无水乙醇洗涤后，60℃烘干，然后研磨，记为固体B；称取壳聚糖粉末分散在醋酸溶液中，搅拌使壳聚糖充分溶解，而后向该壳聚糖醋酸溶液中加入固体B，并搅拌，记为凝胶C；将凝胶C置于60℃恒温水浴锅中老化3d，每8h用无水乙醇置换一次，结束后烘干焙烧，过筛，即得改性壳聚糖气凝胶。
A modified chitosan airgel and its preparation method and application, weigh LaCl 3 • 7H 2 O, ZrOCl 2 • 8H 2 O, dissolve in deionized water, stir in a water bath, and drop NaOH solution, Continue to stir; then age at a constant temperature of 60°C, wash with deionized water and ethanol three times respectively, and record it as solution A; weigh the bentonite raw material and dissolve it in deionized water, and drop solution A into the bentonite slurry at a constant temperature of 60°C, Stir continuously, continue stirring after the dropwise addition, and then age under constant temperature conditions. The aged pillared products are separated by centrifugation, washed with deionized water and absolute ethanol, dried at 60°C, and then ground, recorded as Solid B; take chitosan powder and disperse it in acetic acid solution, stir to make chitosan fully dissolve, then add solid B to the chitosan acetic acid solution, and stir, and record it as gel C; put gel C Aged in a constant temperature water bath at 60°C for 3 days, replaced with absolute ethanol every 8 hours, dried and roasted after completion, and sieved to obtain the modified chitosan airgel.
Description
Technical Field
The invention relates to the field of wastewater treatment, in particular to a modified chitosan aerogel and a preparation method and application thereof.
Background
Eutrophication of surface water bodies has become one of the most prominent water environment problems faced by China at present, and phosphorus is one of key limiting factors for causing the eutrophication of surface water bodies, and can play an important role in regulating and controlling the eutrophication state of the surface water bodies. Sources of phosphorus in the surface water bodies include the excretion of exogenous phosphorus sources and the release of endogenous phosphorus sources. Therefore, in order to control eutrophication of surface water, it is necessary to remove phosphorus from an exogenous phosphorus source such as phosphorus-containing wastewater by effective means. The chitosan has no toxicity and is environment-friendly, and no secondary pollution is caused after the adsorption of the wastewater, so that the chitosan is an ideal high-efficiency adsorbent. However, the chemical properties are unstable, and the chitosan is required to be modified because the chitosan is dissolved in an acidic solution and separated out in an alkaline solution, so that a polymer compound which has stable structural properties and is easy to settle and filter is prepared. Lanthanum is a rich rare earth element and is considered to be environmentally friendly and relatively inexpensive. It can exhibit a specific affinity for phosphate even at a trace level. Accordingly, there is increasing interest in lanthanum-containing phosphorus adsorbent materials. One material widely used for chemical lake remediation is Phoslock, a commercial product developed by CISRO in australia. Studies have shown that La loading on the support can enhance the removal of phosphate from aqueous solutions. If lanthanum and zirconium are used in combination to modify bentonite, the synthesized lanthanum-zirconium modified bentonite may also be used for controlling the release of phosphorus in the sediment. The aerogel is a solid material with a special three-dimensional nano porous structure and filled with air medium, the special structure endows the aerogel with excellent properties such as low density, high porosity, high specific surface area and the like, and in theory, the rare earth/chitosan aerogel has the commonality of both the aerogel and the rare earth compound, and for the aerogel, the rare earth/chitosan aerogel is a relatively new field, the development of the properties and the application of the aerogel is severely limited due to insufficient preparation process, so that the research of the preparation process and the obtainment of the lanthanum-based rare earth composite chitosan aerogel have important practical significance. Therefore, the lanthanum-zirconium modified bentonite is combined with the chitosan aerogel, so that the adsorption performance of the lanthanum-zirconium modified bentonite can be enhanced, the difficult problems of difficult recovery after adsorption and the like are solved, the mechanical performance of the aerogel can be enhanced, the selective absorption of phosphorus in wastewater is enhanced, the cost of the phosphorus removal adsorbent is reduced, and the market demand is met.
Disclosure of Invention
The technical problems to be solved are as follows: aiming at the technical problems, the invention provides a modified chitosan aerogel and a preparation method and application thereof. The aerogel has large specific surface area and high porosity, and the La load can improve the efficient selective adsorption of the aerogel to phosphorus, on the basis, the adsorption performance of the aerogel to phosphorus can be improved by doping a small amount of Zr, and meanwhile, the cyclic desorption performance of the aerogel material is improved, so that the aerogel material is greatly utilized, the bentonite inorganic material is introduced, the cost is greatly reduced, and the market economic requirement is met.
The technical scheme is as follows: the preparation method of the modified chitosan aerogel comprises the following preparation steps: (1) Weighing LaCl 3 •7H 2 O，ZrOCl 2 •8H 2 O, dissolved in deionized water, wherein the molar ratio n (La): n (Zr) = (2-8): 1, is stirred at the water bath temperature of 60 ℃, and NaOH solution is added dropwise, wherein the molar ratio n (OH) - ): n(La 3+ +Zr 4+ ) 1 stirring is continued for 2h; aging at 60 ℃ for 48 hours, washing with deionized water and ethanol for three times respectively, and marking as a solution A; (2) Weighing bentonite raw material, dissolving in 100mL deionized water, dripping solution A into bentonite ore pulp at 80deg.C, and continuously stirring, wherein n (La 3+ +Zr 4+ ): m (bentonite) =1 mmol/g-20mmol/g, continuing stirring for 2h after finishing dripping, then aging for 48h under the constant temperature condition of 60 ℃, centrifugally separating the aged pillared product, washing with deionized water and absolute ethyl alcohol, drying at 60 ℃, grinding for 100 meshes, and marking as solid B; (3) Weighing chitosan powder, dispersing in 100mL of 1wt.% acetic acid solution, stirring to fully dissolve chitosan, adding solid B into the chitosan acetic acid solution, stirring for 2h, and marking as gel C; (4) Aging gel C in a water bath at 60deg.C for 3d with anhydrous water every 8 hrAnd (3) replacing the ethanol once, drying at 60 ℃ after the completion of the replacement, roasting for 3 hours at 500 ℃, and sieving to obtain the modified chitosan aerogel.
Preferably, in the step (1), the molar ratio n (La): n (Zr) =4:1.
Preferably, the molar ratio n (OH) in step (1) - ): n(La 3+ +Zr 4+ ) =2:1, stirring time was 2h.
Preferably, the deionized water and absolute ethanol are washed for not less than 3 times in the step (1),
preferably, the molar ratio n (La 3+ +Zr 4+ ): m (bentonite) =10 mmol/g, stirring time is 2h.
Preferably, in the step (3), m (chitosan): m (bentonite) =1:1, the stirring time is 2h, and the gel time is 20-30min.
Preferably, the roasting temperature in the step (4) is 500 ℃, and the roasting time is 3 hours.
The modified chitosan aerogel prepared by the preparation method is prepared.
The application of the modified chitosan aerogel in preparing the dephosphorization adsorbent.
The beneficial effects are that: 1. according to the invention, chitosan aerogel is selected as a support, and the high adsorption performance of the aerogel, the specific affinity of lanthanum and zirconium to phosphorus and the strong ion exchange performance of bentonite are utilized to enhance the removal effect of phosphorus in wastewater. 2. The waste is recycled, the chitosan is derived from a plurality of wastes such as shrimp shells, and the environment pollution caused by biomass materials can be effectively solved by extracting the chitosan in the wastes to prepare aerogel. 3. The aerogel not only expands the application of the phosphorus locking agent, but also can improve the high load rate of the active site of the aerogel by introducing bentonite, thereby enhancing the high-efficiency adsorption performance of the aerogel. Meanwhile, the chitosan aerogel can reduce the swelling performance of bentonite in water, and can better adsorb phosphorus-containing substances in wastewater.
Drawings
FIG. 1 shows the removal efficiency of phosphorus with different adsorbents;
FIG. 2 shows the adsorption amount of phosphorus by different adsorbents.
Detailed Description
The present invention will be further described in detail with reference to the following examples, but the present invention is not limited thereto.
Example 1
(1) Weighing LaCl 3 •7H 2 O，ZrOCl 2 •8H 2 O, dissolving in deionized water, wherein the molar ratio is n (La): n (Zr) =4:1, and stirring at the water bath temperature of 60 ℃;
(2) Dropwise adding NaOH solution, wherein the molar ratio is n (OH) - ): n(La 3+ +Zr 4+ ) Stirring was continued for 2h, =2:1. Aging at 60 ℃ for 48 hours, washing with deionized water and ethanol for three times respectively, and marking as a solution A;
(3) Weighing bentonite raw material, dissolving in 100mL deionized water, and dripping the solution A into bentonite ore pulp at constant temperature of 80 ℃, wherein the molar ratio is n (La 3+ +Zr 4+ ) M (bentonite) =10 mmol/g, continuously stirring;
(4) Stirring for 2h after dripping, aging at 60deg.C for 48h, centrifuging, washing with deionized water and absolute ethanol for three times, oven drying at 60deg.C, grinding to 100 mesh, and recording as solid B;
(5) The chitosan was weighed and dispersed in 100ml of a 1wt.% acetic acid solution, stirred to make the chitosan fully dissolved, then solid B was added to the chitosan acetic acid solution, wherein the mass ratio was m (chitosan): m (bentonite) =1:1, and stirred for 2h, denoted gel C.
(6) And (3) aging the gel C in a water bath kettle with constant temperature of 60 ℃ for 3d, replacing every 8h with absolute ethyl alcohol, drying at 60 ℃ after the gel C is finished, roasting at 500 ℃ for 3h, and sieving to form the LaZr/Bt@CS aerogel adsorption material.
The adsorption material is added in the following manner: the LaZr/Bt@CS aerogel adsorption material is added according to the dosage of 0.3g/L, firstly, a simulated phosphorus wastewater experiment is carried out, then a 0.45 mu m filter membrane is used for carrying out ultraviolet absorption measurement on phosphorus content in the solution, and the adsorbent on the filter cake is dried and then a desorption experiment is carried out in a NaOH solution.
Example 2
(1) LaCl is taken 3 •7H 2 O，ZrOCl 2 •8H 2 O, dissolving in 100mL deionized water, wherein the molar ratio is n (La): n (Zr) =4:1, and stirring at the water bath temperature of 60 ℃;
(2) Dropwise adding NaOH solution, wherein the molar ratio is n (OH) - ):n(La 3+ +Zr 4+ ) Stirring was continued for 2h, =2:1. Then aging for 48 hours at constant temperature, washing with deionized water and ethanol for three times respectively, and marking as a solution A;
(3) Weighing bentonite raw material, dissolving in 100mL deionized water, and dripping the solution A into bentonite ore pulp at constant temperature of 80 ℃, wherein the molar ratio is n (La 3+ +Zr 4+ ) M (bentonite) =10 mmol/g, continuously stirring;
(4) After the dripping is finished, stirring is continued for 2 hours, then aging is carried out for 48 hours under the constant temperature condition of 60 ℃, the aged pillared product is centrifugally separated, washed by deionized water and absolute ethyl alcohol for three times, then dried in a blast drying oven of 60 ℃, and then ground to 100 meshes, and the solid B is marked;
(5) Dispersing chitosan in 100mL of 1wt.% acetic acid solution, stirring overnight to fully dissolve the chitosan, adding solid B into the chitosan acetic acid solution, wherein the mass ratio of m (chitosan): m (bentonite) =1:0.75, stirring for 2h, and marking as gel C;
(6) And (3) placing the gel C in a constant-temperature water bath kettle at 60 ℃ for aging for 3 days, replacing every 8 hours with absolute ethyl alcohol, drying at 60 ℃ after the gel C is finished, roasting at 500 ℃ for 3 hours, and grinding to form the LaZr/Bt@CS aerogel adsorption material.
The adsorption material is added in the following manner: the LaZr/Bt@CS aerogel adsorption material is added according to the dosage of 0.3g/L, firstly, a simulated phosphorus wastewater experiment is carried out, then a 0.45 mu m filter membrane is used for carrying out ultraviolet absorption measurement on phosphorus content in the solution, and the adsorbent on the filter cake is dried and then a desorption experiment is carried out in a NaOH solution.
Example 3
(1) LaCl is taken 3 •7H 2 O，ZrOCl 2 •8H 2 O, dissolved in 100mL deionized water, wherein the molar ratio is n (La): n (Zr) =4:1, at the water bath temperatureStirring at 60 ℃;
(2) Dropwise adding NaOH solution, wherein the molar ratio is n (OH) - ):n(La 3+ +Zr 4+ ) Stirring was continued for 2h, =2:1. Aging at 60 ℃ for 48 hours, washing with deionized water and ethanol for three times respectively, and marking as a solution A;
(3) Weighing bentonite raw material, dissolving in 100mL deionized water, and dripping the solution A into bentonite ore pulp at constant temperature of 80 ℃, wherein the molar ratio is n (La 3+ +Zr 4+ ) M (bentonite) =10 mmol/g, continuously stirring;
(4) Stirring for 2h after dripping, aging at 60deg.C for 48h, centrifuging, washing with deionized water and absolute ethanol for three times, oven drying at 60deg.C, grinding to 100 mesh, and recording as solid B;
(5) Dispersing chitosan in 100mL of 1wt.% acetic acid solution, stirring to fully dissolve the chitosan, adding solid B into the chitosan acetic acid solution, wherein the mass ratio of m (chitosan): m (bentonite) =1:0.5, stirring for 2h, and marking as gel C;
(6) And (3) placing the gel C in a constant-temperature water bath kettle at 60 ℃ for aging for 3 days, replacing every 8 hours with absolute ethyl alcohol, drying at 60 ℃ after the gel C is finished, roasting at 500 ℃ for 3 hours, and grinding to form the LaZr/Bt@CS aerogel adsorption material.
The adsorption material is added in the following manner: the LaZr/Bt@CS aerogel adsorption material is added according to the dosage of 0.3g/L, firstly, a simulated phosphorus wastewater experiment is carried out, then a 0.45 mu m filter membrane is used for carrying out ultraviolet absorption measurement on phosphorus content in the solution, and the adsorbent on the filter cake is dried and then a desorption experiment is carried out in a NaOH solution.
Comparative scheme 1
LaZr adsorption material was prepared according to the method in example L, and was subjected to a simulated phosphorus wastewater experiment at first according to the dosage of 0.3g/L, then through a 0.45 μm filter membrane, the solution was subjected to ultraviolet absorption measurement of phosphorus content, the adsorbent on the filter cake was dried, and the desorption experiment was performed in NaOH solution.
LaZr/Bt adsorbing material was prepared according to the method in example 2, and was subjected to a simulated phosphorus wastewater experiment according to the amount of 0.3g/L, then the phosphorus content was measured by ultraviolet absorption through a 0.45 μm filter membrane, the adsorbent on the filter cake was dried, and the desorption experiment was performed in NaOH solution.
Comparative scheme 3
LaZr@CS aerogel adsorbing material is prepared according to the method in example 3, la-Zr@CS aerogel adsorbing material is added according to the adding amount of 0.3g/L, a simulated phosphorus wastewater experiment is firstly carried out, then a 0.45 mu m filter membrane is used for carrying out ultraviolet absorption measurement on phosphorus content in the solution, the adsorbent on the filter cake is dried, and a desorption experiment is carried out in NaOH solution.
As described above, although the present invention has been shown and described with reference to certain preferred embodiments, it is not to be construed as limiting the invention itself. Various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (3)
1. The preparation method of the modified chitosan aerogel is characterized by comprising the following steps: (1) Weighing LaCl 3 •7H 2 O，ZrOCl 2 •8H 2 O, dissolving in deionized water, wherein the molar ratio n (La): n (Zr) =4:1, stirring at the water bath temperature of 60 ℃, and dropwise adding NaOH solution, wherein the molar ratio n (OH) - ): n(La 3+ +Zr 4+ ) Stirring was continued for 2h =2:1; aging at 60 ℃ for 48 hours, washing with deionized water and ethanol for three times respectively, and marking as a solution A; (2) Weighing bentonite raw material, dissolving in 100mL deionized water, dripping solution A into bentonite ore pulp at 80deg.C, and continuously stirring, wherein n (La 3+ +Zr 4+ ): m (bentonite) =10 mmol/g, continuing stirring for 2 hours after finishing dripping, aging for 48 hours at a constant temperature of 60 ℃, centrifugally separating the aged pillared product, washing with deionized water and absolute ethyl alcohol, drying at 60 ℃, grinding for 100 meshes, and marking as solid B; (3) Dispersing chitosan powder in 100mL 1wt.% acetic acid solution, stirring to dissolve chitosan completely, and adding into the chitosan acetic acid solutionSolid B, wherein the mass ratio is m (chitosan): m (bentonite) =1:1, and stirred for 2h, noted gel C; (4) And (3) placing the gel C in a constant-temperature water bath kettle at 60 ℃ for aging for 3 days, replacing every 8 hours with absolute ethyl alcohol, drying at 60 ℃ after the gel C is finished, roasting at 500 ℃ for 3 hours, and sieving to obtain the modified chitosan aerogel.
2. The modified chitosan aerogel prepared by the preparation method of claim 1.
3. The use of the modified chitosan aerogel of claim 2 in the preparation of a dephosphorizing adsorbent.
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| CN105712400B (en) * | 2016-04-27 | 2017-05-03 | 上海应用技术学院 | Method for preparing zirconia aerogel material |
| CN107754756A (en) * | 2017-11-10 | 2018-03-06 | 四川理工学院 | A kind of dephosphorization preparation method for bentonite |
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| CN111468076A (en) * | 2020-04-08 | 2020-07-31 | 广州大学 | Chitosan-zirconium composite gel spheres modified by amino-rich compounds and their preparation and application |
| CN112337427B (en) * | 2020-10-15 | 2022-07-19 | 四川轻化工大学 | A kind of preparation method of La@Zr@SiO2@bentonite composite phosphorus removal adsorbent |
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