CN115138339A - Montmorillonite-chitosan-hydroxyl iron composite material and preparation method thereof - Google Patents
Montmorillonite-chitosan-hydroxyl iron composite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a montmorillonite-chitosan-hydroxyl iron composite material and a preparation method thereof, and relates to the technical field of water pollutant treatment. The invention uses chitosan to carry out intercalation modification on acid-treated montmorillonite, and then chitosan intercalation montmorillonite and FeCl 3 And combining to obtain the montmorillonite-chitosan-hydroxyl iron composite material. The montmorillonite-chitosan-hydroxyl iron composite material has the advantages of simple preparation process, low cost, no adverse effect on the environment, no secondary pollution to water, high material adsorption rate and high efficiency, and can remove arsenic and antimony in waterThe removal rate reaches more than 95 percent.
Description
Technical Field
The invention relates to the technical field of water pollutant treatment, in particular to a montmorillonite-chitosan-hydroxyl iron composite material and a preparation method thereof.
Background
Pollution remediation of arsenic and antimony in water bodies is always a research hotspot at home and abroad, and antimony is usually associated with arsenic, and the arsenic and the antimony have similar earth environment behaviors. Arsenite [ As (III) ], antimonite [ Sb (III) ], and have greater toxicity, solubility, mobility, and bioavailability than arsenate [ As (V) ], antimonate [ Sb (V) ]. Therefore, the treatment and adsorption of arsenic and antimony pollutant radicals in the water body are crucial to the pollutant treatment of the water body. However, the existing arsenic and antimony pollutant adsorbing materials for the water body generally have the problems of high cost, low adsorption efficiency, easy secondary pollution of the water body and the like. Therefore, how to overcome the above problems and prepare an arsenic and antimony pollutant adsorbing material which is special for water, has low cost, high adsorption efficiency, is environment-friendly and does not cause secondary pollution is a technical problem to be solved urgently at present.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a montmorillonite-chitosan-hydroxyl iron composite material, which specifically comprises the following steps:
(1) Mixing montmorillonite and hydrochloric acid to react under the condition of stirring, cooling and filtering after the reaction is finished, washing a reactant with deionized water to remove residual hydrochloric acid, drying and grinding the reactant after the washing is finished, and sieving the reactant with a 200-mesh sieve to obtain montmorillonite powder;
(2) Mixing chitosan and 1wt% acetic acid solution according to the material-liquid ratio of 1g: mixing 40mL of the mixture, fully stirring the mixture to dissolve the mixture to prepare a chitosan solution, and mixing montmorillonite powder and deionized water according to a material-liquid ratio of 1g: mixing at a ratio of 20mL, and fully stirring to uniformly disperse the mixture in water to obtain a montmorillonite suspension; carrying out intercalation modification on the chitosan solution and the montmorillonite suspension under the condition of continuous stirring, cooling to room temperature after modification is finished, centrifugally separating out a solid from a reactant at the rotating speed of 8000r/min, washing with deionized water, drying the product at 105 ℃ for 12 hours, grinding the dried solid into powder, and sieving with a 200-mesh sieve to obtain chitosan intercalation montmorillonite;
(3) Mixing chitosan intercalation montmorillonite and deionized water according to a material-liquid ratio of 1g: mixing at a ratio of 50mL, stirring to disperse uniformly in water to obtain chitosan intercalation montmorillonite suspension, and weighing FeCl 3 Dissolving the solid in deionized water to obtain FeCl 3 Solution, under the condition of rapid stirring, feCl 3 Quickly dripping the solution into the chitosan intercalation montmorillonite suspension, and continuously stirring for 5min to obtain chitosan intercalation montmorillonite mixed solution containing iron ions;
and quickly dropwise adding a NaOH solution with the concentration of 0.1mol/L into the mixed solution, converting iron ions into hydroxyl iron by using the action of sodium hydroxide, after dropwise adding, quickly heating the system under the condition of continuous stirring, reacting, cooling to room temperature after reaction, carrying out suction filtration, washing residual NaOH solution in the solid product by using deionized water, drying the product after washing, grinding, and sieving by using a 200-mesh sieve to obtain the montmorillonite-chitosan-hydroxyl iron composite material.
Further, the hydrochloric acid concentration in the step (1) is 2mol/L, and the material-liquid ratio of montmorillonite to hydrochloric acid is 1g:20mL.
Further, in the step (1), the reaction temperature is 70-90 ℃, the reaction time is 8 hours, the drying temperature is 105 ℃, and the drying time is 12 hours.
Further, the weight ratio of the montmorillonite suspension to the chitosan solution in the step (2) is 105:102.5.
further, the intercalation modification temperature in the step (2) is 70-90 ℃, and the intercalation modification time is 10 hours.
Further, feCl is added in the step (3) 3 The concentration of the solution is 0.0358-0.1432 mol/L, and the weight ratio of the ferric chloride solution to the chitosan intercalation montmorillonite suspension is 50.48-51.94: 102.
further, the molar ratio of NaOH to Fe in the step (3) is 1:1 to 1.
Further, in the step (3), the reaction temperature is 70-90 ℃, the reaction time is 4h, the drying temperature is 105 ℃, and the drying time is 12h.
The invention also provides a montmorillonite-chitosan-hydroxyl iron composite material prepared by the method.
Another object of the present invention is to provide the use of the montmorillonite-chitosan-iron hydroxide composite material in the adsorption of heavy metals in water, including but not limited to arsenic and antimony.
Compared with the prior art, the invention has the beneficial technical effects that:
(1) The main raw materials adopted by the invention are montmorillonite and chitosan, the montmorillonite is a natural clay mineral material with large reserves on the earth, and the chitosan is a product obtained by deacetylating chitin widely existing in the nature, so the price of the montmorillonite and the chitosan is low, in addition, the preparation process of the montmorillonite-chitosan-hydroxyl iron composite material has mild conditions, no special requirements on production equipment are required, and the preparation cost of the montmorillonite-chitosan-hydroxyl iron composite material is further obviously reduced;
(2) The montmorillonite and the chitosan which are adopted by the invention are environment-friendly materials, the environment pollution is not caused by the montmorillonite and the chitosan, organic solvents or other toxic and harmful substances are not used in the preparation process of the montmorillonite-chitosan-hydroxyl iron composite material, and actual detection proves that the montmorillonite-chitosan-hydroxyl iron composite material can not release a large amount of Fe into water in the process of adsorbing arsenic and antimony, so that the problems of solvent residue and secondary pollution are avoided;
(3) The montmorillonite-chitosan-iron hydroxide composite material has the characteristics of high adsorption rate and high efficiency, the removal rate of arsenic and antimony in a water body is up to more than 80% (within 10 min), and the final removal rate is higher than 95%.
Drawings
The invention is further illustrated in the following description with reference to the drawings.
FIG. 1 is an XRD spectrum of the invention.
Detailed Description
The invention provides a preparation method of a montmorillonite-chitosan-hydroxy iron composite material, which comprises the following steps:
(1) Mixing montmorillonite and hydrochloric acid to react under the condition of stirring, cooling and filtering after the reaction is finished, washing a reactant with deionized water to remove residual hydrochloric acid, drying and grinding the reactant after the washing is finished, and sieving the reactant with a 200-mesh sieve to obtain montmorillonite powder;
(2) Mixing chitosan and 1wt% acetic acid solution according to the material-liquid ratio of 1g: mixing 40mL of the mixture, fully stirring the mixture to dissolve the mixture to prepare a chitosan solution, and mixing montmorillonite powder and deionized water according to a material-liquid ratio of 1g: mixing at a ratio of 20mL, and fully stirring to uniformly disperse the mixture in water to obtain a montmorillonite suspension; carrying out intercalation modification on the chitosan solution and the montmorillonite suspension under the condition of continuous stirring, cooling to room temperature after modification is finished, centrifugally separating out a solid from a reactant at the rotating speed of 8000r/min, washing with deionized water, drying the product at 105 ℃ for 12 hours, grinding the dried solid into powder and sieving with a 200-mesh sieve to obtain chitosan intercalation montmorillonite;
(3) Mixing chitosan intercalation montmorillonite and deionized water according to a material-liquid ratio of 1g: mixing at a ratio of 50mL, stirring to disperse uniformly in water to obtain chitosan intercalation montmorillonite suspension, and weighing FeCl 3 Dissolving the solid in deionized water to obtain FeCl 3 Solution, under the condition of rapid stirring, feCl 3 Quickly dripping the solution into the chitosan intercalation montmorillonite suspension, and continuously stirring for 5min to obtain chitosan intercalation montmorillonite mixed solution containing iron ions;
and quickly dropwise adding a 0.1mol/L NaOH solution into the mixed solution, converting iron ions into hydroxyl iron by utilizing the action of sodium hydroxide, after dropwise adding, quickly heating the system under the condition of continuous stirring, reacting, cooling to room temperature after the reaction is finished, performing suction filtration, washing residual NaOH solution in the solid product by using deionized water, drying the product after washing, grinding, and sieving by using a 200-mesh sieve to obtain the montmorillonite-chitosan-hydroxyl iron composite material.
In one embodiment, the hydrochloric acid concentration in the step (1) is 2mol/L, and the feed-liquid ratio of montmorillonite to hydrochloric acid is 1g:20mL.
In one embodiment, in the step (1), the reaction temperature is 70-90 ℃, the reaction time is 8 hours, the drying temperature is 105 ℃, and the drying time is 12 hours.
In one embodiment, the weight ratio of the montmorillonite suspension to the chitosan solution in step (2) is 105:102.5.
in one embodiment, the intercalation modification temperature in the step (2) is 70-90 ℃, and the intercalation modification time is 10h.
In one embodiment, feCl in said step (3) 3 The concentration of the solution is 0.0358-0.1432 mol/L, the weight ratio of the ferric chloride solution to the chitosan intercalation montmorillonite suspension is 50.48-51.94: 102.
in one embodiment, the molar ratio of NaOH to Fe in step (3) is 1:1 to 1.
In one embodiment, in the step (3), the reaction temperature is 70-90 ℃, the reaction time is 4 hours, the drying temperature is 105 ℃, and the drying time is 12 hours.
The invention also provides a montmorillonite-chitosan-hydroxyl iron composite material prepared by the method.
Another object of the present invention is to provide the use of the montmorillonite-chitosan-iron hydroxide composite material in adsorbing heavy metals including but not limited to arsenic and antimony in water.
The technical solution provided by the present invention is further illustrated by the following examples.
Example 1
A preparation method of a montmorillonite-chitosan-hydroxyl iron composite material with the chitosan dosage of 2.5g and the iron load of 15wt% comprises the following steps:
(1) Adding 10g of montmorillonite into 200mL of hydrochloric acid with the concentration of 2mol/L, stirring for 8h at 80 ℃, after finishing and cooling, carrying out suction filtration on a reactant, washing away residual acid by deionized water, then placing the reactant in an oven for drying for 12h at 105 ℃, grinding the dried montmorillonite into powder, and sieving the powder with a 200-mesh sieve;
(2) Adding 2.5g of chitosan into 100mL of 1% acetic acid solution, stirring to fully dissolve the chitosan to prepare a chitosan solution, adding 5g of montmorillonite treated by hydrochloric acid into 100mL of deionized water, stirring and dispersing, adding the chitosan solution into a montmorillonite suspension, stirring for 10 hours at 80 ℃, after finishing and cooling, centrifugally separating out solid from a reactant at the rotating speed of 8000r/min, washing with deionized water, placing the obtained product in a drying oven, drying for 12 hours at 105 ℃, grinding the dried solid into powder, and sieving with a 200-mesh sieve to obtain chitosan intercalated montmorillonite;
(3) Adding the chitosan intercalated montmorillonite into deionized water, stirring and dispersing to obtain montmorillonite suspension, and preparing FeCl with the concentration of 0.1074mol/L 3 Solution, under rapid stirring, feCl 3 The solution was quickly added dropwise to the montmorillonite suspension, wherein the weight ratio of montmorillonite suspension to chitosan solution was 105:102.5, continuously stirring for 5min, and then mixing according to the molar ratio of NaOH to Fe of 3:1, quickly dropwise adding a 0.1mol/L NaOH solution, continuously stirring and quickly heating to 80 ℃ to react for 4 hours at the temperature after dropwise adding is finished, filtering the reactant and washing away residual NaOH by deionized water after the reaction is finished and cooled, then placing the reactant in a drying oven to dry for 12 hours at 105 ℃, grinding the dried montmorillonite into powder and sieving the powder by a 200-mesh sieve to obtain the montmorillonite-chitosan-hydroxyl iron composite material.
The adsorption performance of the montmorillonite-chitosan-hydroxyl iron composite material is detected by an arsenic and antimony adsorption experiment, and the method comprises the following steps:
weighing 15mg of montmorillonite-chitosan-hydroxyl iron composite material, adding into a PET bottle with the capacity of 50mL, respectively adding 20mL of arsenic and antimony solutions with the pH =3 and the concentration of 10mg/L prepared in advance into the bottle, placing the bottle into a water bath oscillator, oscillating for 4h at the oscillation rate of 200r/min and the temperature of 25 ℃, taking out, respectively filtering the arsenic and antimony solutions after treatment by using a disposable filter with the pore diameter of 0.22 mu m, and measuring the concentrations of As (III), as (V), sb (III) and Sb (V) in the filtrate by adopting an ICP-OES spectrometer.
The experimental results are as follows: the removal rate of As (III), as (V), sb (III) and Sb (V) of the montmorillonite-chitosan-hydroxyl iron composite material is respectively 96.65%, 99.04%, 98.40% and 99.64%.
Example 2
A preparation method of a montmorillonite-chitosan-hydroxyl iron composite material with chitosan dosage of 2.5g and iron load of 10% comprises the following steps:
(1) Adding 10g of montmorillonite into 200mL of hydrochloric acid with the concentration of 2mol/L, stirring for 8h at 80 ℃, after finishing and cooling, carrying out suction filtration on a reactant, washing away residual acid by deionized water, then placing the reactant in an oven for drying for 12h at 105 ℃, grinding the dried montmorillonite into powder, and sieving the powder with a 200-mesh sieve;
(2) Adding 2.5g of chitosan into 100mL of 1% acetic acid solution, stirring to fully dissolve the chitosan, preparing a chitosan solution, adding montmorillonite subjected to hydrochloric acid treatment into 100mL of deionized water, stirring and dispersing, adding the chitosan solution into a montmorillonite suspension, stirring for 10 hours at 80 ℃, after finishing and cooling, centrifugally separating out solids from reactants at a rotating speed of 8000r/min, washing with deionized water, placing the obtained product in a drying oven, drying for 12 hours at 105 ℃, grinding the dried solids into powder, and sieving with a 200-mesh sieve to obtain chitosan intercalated montmorillonite;
(3) Adding the chitosan intercalated montmorillonite into deionized water, stirring and dispersing to obtain montmorillonite suspension, and preparing FeCl with the concentration of 0.0716mol/L 3 Solution, under rapid stirring, feCl 3 The solution was quickly added dropwise to the montmorillonite suspension, wherein the weight ratio of montmorillonite suspension to chitosan solution was 105:102.5, continuously stirring for 5min, and then mixing according to the molar ratio of NaOH to Fe of 3:1, quickly dripping 0.1mol/L NaOH solution, continuously stirring and quickly heating to 80 DEG CAnd reacting for 4 hours at the temperature, after the reaction is finished and cooled, carrying out suction filtration on the reactant, washing away residual NaOH by using deionized water, then placing the reactant in a drying oven, drying for 12 hours at 105 ℃, grinding the dried montmorillonite into powder, and sieving the powder by using a 200-mesh sieve to obtain the montmorillonite-chitosan-hydroxyl iron composite material.
The adsorption performance of the montmorillonite-chitosan-hydroxyl iron composite material is detected by an arsenic and antimony adsorption experiment, and the method comprises the following steps:
weighing 10mg of montmorillonite-chitosan-iron hydroxide composite material, adding the montmorillonite-chitosan-iron hydroxide composite material into a PET bottle with the capacity of 50mL, respectively adding 20mL of arsenic and antimony solutions with the pH =3 and the concentration of 10mg/L into the bottle, placing the bottle into a water bath oscillator, oscillating for 4h under the conditions of the oscillation rate of 200r/min and the temperature of 25 ℃, taking out the bottle, respectively filtering the arsenic and antimony solutions after treatment by using a disposable filter with the pore diameter of 0.22 mu m, and measuring the concentrations of As (III), as (V), sb (III) and Sb (V) in the filtrate by using an ICP-OES spectrometer.
The experimental results are as follows: the removal rates of the montmorillonite-chitosan-iron hydroxide composite material on As (III), as (V), sb (III) and Sb (V) are respectively 97.91%, 96.50%, 95.34% and 99.81%.
Test example 1
The montmorillonite-chitosan-iron oxyhydroxide composite material prepared in example 1 was fully ground and sieved through a 200 mesh sieve, and then placed in an oven to be dried at 105 ℃ for 4 hours to remove moisture therefrom, characterized by using an X-ray diffractometer of Bruker D8Advance, with a test scan speed of 5 °/min and an angle of 3 to 70 °, and the results are shown in fig. 1.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (10)
1. A method for preparing a montmorillonite-chitosan-hydroxyl iron composite material is characterized by comprising the following steps:
(1) Mixing montmorillonite and hydrochloric acid to react under the condition of stirring, cooling and filtering after the reaction is finished, washing the reactant with deionized water to remove residual hydrochloric acid, drying and grinding the reactant after the washing is finished, and sieving the reactant with a 200-mesh sieve to obtain montmorillonite powder;
(2) Mixing chitosan and 1wt% acetic acid solution according to the material-liquid ratio of 1g: mixing 40mL of the mixture, fully stirring the mixture to dissolve the mixture to prepare a chitosan solution, and mixing montmorillonite powder and deionized water according to a material-liquid ratio of 1g: mixing at a ratio of 20mL, and fully stirring to uniformly disperse the mixture in water to obtain a montmorillonite suspension; carrying out intercalation modification on the chitosan solution and the montmorillonite suspension under the condition of continuous stirring, cooling to room temperature after modification is finished, centrifugally separating out a solid from a reactant at the rotating speed of 8000r/min, washing with deionized water, drying the product at 105 ℃ for 12 hours, grinding the dried solid into powder and sieving with a 200-mesh sieve to obtain chitosan intercalation montmorillonite;
(3) Mixing chitosan intercalation montmorillonite and deionized water according to a material-liquid ratio of 1g: mixing at a ratio of 50mL, stirring to disperse uniformly in water to obtain chitosan intercalation montmorillonite suspension, and weighing FeCl 3 The solid is dissolved in 50mL deionized water to obtain FeCl 3 Solution, under the condition of rapid stirring, feCl 3 Quickly dripping the solution into the chitosan intercalation montmorillonite suspension, and continuously stirring for 5min to obtain chitosan intercalation montmorillonite mixed solution containing iron ions;
and quickly dropwise adding a 0.1mol/L NaOH solution into the mixed solution, after dropwise adding, quickly heating the system under the condition of continuous stirring, reacting, cooling to room temperature after reaction, carrying out suction filtration, washing residual NaOH solution in the solid product with deionized water, drying the product after washing, grinding, and sieving with a 200-mesh sieve to obtain the montmorillonite-chitosan-hydroxyl iron composite material.
2. The method for preparing the montmorillonite-chitosan-hydroxy-iron composite material according to claim 1, wherein the hydrochloric acid concentration in the step (1) is 2mol/L, and the feed-liquid ratio of montmorillonite to hydrochloric acid is 1g:20mL.
3. The method for preparing the montmorillonite-chitosan-iron hydroxide composite material according to claim 1, wherein in the step (1), the reaction temperature is 70-90 ℃, the reaction time is 8 hours, the drying temperature is 105 ℃, and the drying time is 12 hours.
4. The method for preparing a montmorillonite-chitosan-iron oxyhydroxide composite material according to claim 1, wherein the weight ratio of the montmorillonite suspension to the chitosan solution in the step (2) is 105:102.5.
5. the method for preparing the montmorillonite-chitosan-iron oxyhydroxide composite material according to claim 1, wherein the intercalation modification temperature in the step (2) is 70-90 ℃, and the intercalation modification time is 10h.
6. The method for preparing the montmorillonite-chitosan-FeOH composite material according to claim 1, wherein FeCl is added in the step (3) 3 The concentration of the solution is 0.0358-0.1432 mol/L, and the weight ratio of the ferric chloride solution to the chitosan intercalation montmorillonite suspension is 50.48-51.94: 102.
7. the method for preparing a montmorillonite-chitosan-hydroxy-iron composite material according to claim 1, wherein the molar ratio of NaOH to Fe in the step (3) is 1:1 to 1.
8. The method for preparing the montmorillonite-chitosan-iron oxyhydroxide composite material according to claim 1, wherein the reaction temperature in the step (3) is 70-90 ℃, the reaction time is 4 hours, the drying temperature is 105 ℃, and the drying time is 12 hours.
9. A montmorillonite-chitosan-hydroxy iron composite material characterized by being prepared by the method of any one of claims 1 to 8.
10. The use of the montmorillonite-chitosan-FeOH composite material according to claim 9, wherein the composite material is used for adsorbing heavy metals in water, and the heavy metals include but are not limited to arsenic and antimony.
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| CN116969758A (en) * | 2022-12-06 | 2023-10-31 | 重庆文理学院 | Preparation method of high-stability zirconia ceramic material |
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