CN111729658A - Preparation method of Cr (III) ion imprinted material based on MCM-41 molecular sieve surface - Google Patents
Preparation method of Cr (III) ion imprinted material based on MCM-41 molecular sieve surface Download PDFInfo
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- CN111729658A CN111729658A CN202010714739.4A CN202010714739A CN111729658A CN 111729658 A CN111729658 A CN 111729658A CN 202010714739 A CN202010714739 A CN 202010714739A CN 111729658 A CN111729658 A CN 111729658A
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- 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
- B01J20/26—Synthetic macromolecular compounds
- B01J20/268—Polymers created by use of a template, e.g. molecularly imprinted polymers
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- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/305—Addition of material, later completely removed, e.g. as result of heat treatment, leaching or washing, e.g. for forming pores
- B01J20/3057—Use of a templating or imprinting material ; filling pores of a substrate or matrix followed by the removal of the substrate or matrix
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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Abstract
The invention discloses a preparation method of a Cr (III) ion imprinted material based on the surface of an MCM-41 molecular sieve. The method takes N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane as a functional monomer, epichlorohydrin as a cross-linking agent and mesoporous MCM-41 as a carrier, and prepares a Cr (III) ion imprinted material based on the surface of the MCM-41 molecular sieve by adopting a surface imprinting method. The mesoporous MCM-41Cr (III) ion imprinting adsorption material has a specific three-dimensional cavity structure, is good in mechanical property, easy to elute, capable of being used for specific identification and selective removal of Cr (III) ions in an aqueous solution, low in cost, environment-friendly and the like.
Description
Technical Field
The invention belongs to the technical field of preparation of environment functional materials, and particularly relates to a preparation method of a Cr (III) ion imprinted material based on the surface of an MCM-41 molecular sieve.
Background
Cr (III) ions have high toxicity, and easily produce enrichment effect on aquatic organisms and human bodies, thereby causing teratogenesis, carcinogenesis and mutagenic three-cause harm. Most of the traditional treatment methods adopt an adsorption method, have the advantages of low cost and simple operation, but lack pertinence and great blindness to target ions, so that research and development of an adsorption material with selective separation to the target ions are particularly important.
The ion imprinting technology is a technology with selective and specific recognition function on target ions, and the ion imprinting polymer is a rigid polymer with cavities with specific shapes and sizes, which is formed by taking anions and cations as templates, reacting with functional monomers through special coordination, complexation or electrostatic interaction and the like, further performing cross-linking polymerization, and removing the template ions by adopting a physical or chemical method. According to the traditional ion imprinting preparation method, recognition sites are distributed in an imprinting material, and a part of the recognition sites are embedded too deeply, so that template ions cannot reach to form failure sites, and the defects of low mass transfer speed and difficult elution exist. The surface ion imprinting technology is a novel ion imprinting technology which is rapidly developed on the basis of the traditional ion imprinting preparation technology, and almost all recognition sites are designed on the surface of a carrier by adopting certain measures, so that the mass transfer effect between the recognition sites and target ions is improved, the elution and recombination of the target ions are facilitated, and the defects of the traditional method are effectively avoided.
The surface ion imprinting technology is used for preparing the imprinting material, and the carrier can increase the surface area, the mechanical strength, the thermal stability and other characteristics of the imprinting polymer to improve the adsorption performance of the imprinting material. The selection of the carrier is particularly important, the MCM-41 mesoporous molecular sieve has the characteristics of large specific surface area, large macroporous volume, large adsorption capacity, high porosity, narrow pore size distribution, rich hydroxyl on the surface, ordered long-range structure, easy control of pore size and the like, can be used for chemical modification, is an ideal imprinted carrier, and the surface imprinted adsorption material synthesized by using the MCM-41 molecular sieve as an imprinted substrate has the advantages of high selectivity and high identification on template ions, low cost and environmental protection.
Disclosure of Invention
The invention aims to provide a preparation method of a Cr (III) ion imprinted material based on the surface of an MCM-41 molecular sieve. The method has the advantages of low cost, environmental protection, high selectivity and high identification on target ions, and the target ions are Cr (III) ions.
The method comprises the following specific steps:
(1) preparation of MCM-41: 1.2g of cetyltrimethylammonium bromide was weighed into a three-necked flask, and at the same time, 90mL of ammonia water and 130mL of distilled water were weighed and added to the three-necked flask. Stirring at 60 ℃ until the cetyltrimethylammonium bromide is completely dissolved. Under the condition of vigorous stirring, slowly dropwise adding 5mL of tetraethoxysilane, then stirring at a constant speed, and reacting for 6 h. Stopping the reaction, pouring out while the reaction is hot, and crystallizing for 3d at room temperature. The solid particles are washed to neutrality and dried. Burning the mixture for 6 hours at 550 ℃ in a muffle furnace to remove hexadecyl trimethyl ammonium bromide to obtain MCM-41;
(2) weighing 0.2-0.3mmol of chromium sulfate hexahydrate solid in a three-necked bottle, adding 10mL of ultrapure water to fully dissolve the chromium sulfate hexahydrate solid, weighing 80-100mL of absolute ethanol, adding the absolute ethanol into the three-necked bottle, uniformly mixing, dropwise adding 2mL of N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, reacting for 1-2h, then adding 1g of MCM-41 obtained in the step (1), condensing and refluxing at 60-80 ℃ for 20h, then adding 1.44mL of epoxy chloropropane, continuing to react for 2-4h, cooling, carrying out suction filtration, and washing for 2-3 times by using the absolute ethanol;
(3) and (3) finally, adding 2mol/L hydrochloric acid in the step (2) to elute for 2-4h at normal temperature, washing with deionized water to be neutral, and drying at 80 ℃ to obtain the MCM-41 molecular sieve surface-based Cr (III) ion imprinted material.
The method has the beneficial effects that the surface imprinting method is adopted, the mesoporous MCM-41 with large specific surface area, good mechanical property and stability and a large number of silicon hydroxyl groups on the surface is used as a carrier, the N- (β -aminoethyl) -gamma-aminopropyltrimethoxysilane is used as a functional monomer, the epichlorohydrin is used as a cross-linking agent, the preparation method of the Cr (III) ion imprinting material based on the MCM-41 molecular sieve surface is prepared through polymerization, and the method is applied to the research on Cr (III) ions, the imprinting material has a removal rate of 93.52 percent on 50mg/L Cr (III) ion solution, has good adsorbability, and can be used for adsorbing Cl (III) ions-、NO3 -、SO4 2-、HPO4 2-The selectivity coefficient of the catalyst can reach more than 1.5, and the catalyst has good selectivity.
Detailed Description
The present invention is further illustrated by the following examples and comparative examples, but the following descriptions are only illustrative of the present invention and are not intended to limit the scope of the present invention.
Example 1:
a method for preparing a Cr (III) ion imprinted material based on the surface of an MCM-41 molecular sieve comprises the following steps:
(1) preparation of MCM-41: 1.2g of cetyltrimethylammonium bromide was weighed into a three-necked flask, and at the same time, 90mL of ammonia water and 130mL of distilled water were weighed and added to the three-necked flask. Stirring at 60 ℃ until the cetyltrimethylammonium bromide is completely dissolved. Under the condition of vigorous stirring, slowly dropwise adding 5mL of tetraethoxysilane, then stirring at a constant speed, and reacting for 6 h. Stopping the reaction, pouring out while the reaction is hot, and crystallizing for 3d at room temperature. The solid particles are washed to neutrality and dried. Burning the mixture for 6 hours at 550 ℃ in a muffle furnace to remove hexadecyl trimethyl ammonium bromide to obtain MCM-41;
(2) weighing 0.2mmol of chromium sulfate hexahydrate solid in a three-necked bottle, adding 10mL of ultrapure water to fully dissolve the chromium sulfate hexahydrate solid, weighing 80-100mL of absolute ethanol, adding the absolute ethanol into the three-necked bottle, uniformly mixing, dropwise adding 2mL of N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, reacting for 1-2h, then adding 1g of MCM-41 obtained in the step (1), condensing and refluxing at 60 ℃ for 20h, then adding 1.44mL of epoxy chloropropane, continuing to react for 2-4h, cooling, carrying out suction filtration, and washing for 2-3 times by using the absolute ethanol;
(3) and (3) finally, adding 2mol/L hydrochloric acid in the step (2) to elute for 2-4h at normal temperature, washing with deionized water to be neutral, and drying at 80 ℃ to obtain the Cr (III) ion imprinting material based on the surface of the MCM-41 molecular sieve. (MCM-41-IIP 1).
Comparative example 1:
the rest of the preparation steps are the same as the example 1, except that chromium sulfate hexahydrate is not added in the step (2), and the MCM-41 molecular sieve non-imprinted adsorption material (MCM-41-NIP1) is prepared.
Example 2:
(1) preparation of MCM-41: 1.2g of cetyltrimethylammonium bromide was weighed into a three-necked flask, and at the same time, 90mL of ammonia water and 130mL of distilled water were weighed and added to the three-necked flask. Stirring at 60 ℃ until the cetyltrimethylammonium bromide is completely dissolved. Under the condition of vigorous stirring, slowly dropwise adding 5mL of tetraethoxysilane, then stirring at a constant speed, and reacting for 6 h. Stopping the reaction, pouring out while the reaction is hot, and crystallizing for 3d at room temperature. The solid particles are washed to neutrality and dried. Burning the mixture for 6 hours at 550 ℃ in a muffle furnace to remove hexadecyl trimethyl ammonium bromide to obtain MCM-41;
(2) weighing 0.25mmol of chromium sulfate hexahydrate solid in a three-necked bottle, adding 10mL of ultrapure water to fully dissolve the chromium sulfate hexahydrate solid, weighing 80-100mL of methanol, adding the methanol into the three-necked bottle, uniformly mixing, dropwise adding 2mL of N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, reacting for 1-2h, then adding 1g of MCM-41 obtained in the step (1), condensing and refluxing at 70 ℃ for 20h, then adding 1.44mL of epoxy chloropropane, continuing to react for 2-4h, cooling, carrying out suction filtration, and washing for 2-3 times by using absolute ethyl alcohol;
(3) and (3) finally, adding 2mol/L hydrochloric acid in the step (2) to elute for 2-4h at normal temperature, washing with deionized water to be neutral, and drying at 80 ℃ to obtain the Cr (III) ion imprinting material based on the surface of the MCM-41 molecular sieve. (MCM-41-IIP 2);
comparative example 2:
the rest of the preparation steps are the same as the example 2, except that chromium sulfate hexahydrate is not added in the step (2), and the MCM-41 molecular sieve non-imprinted adsorption material (MCM-41-NIP2) is prepared.
Example 3:
(1) preparation of MCM-41: 1.2g of cetyltrimethylammonium bromide was weighed into a three-necked flask, and at the same time, 90mL of ammonia water and 130mL of distilled water were weighed and added to the three-necked flask. Stirring at 60 ℃ until the cetyltrimethylammonium bromide is completely dissolved. Under the condition of vigorous stirring, slowly dropwise adding 5mL of tetraethoxysilane, then stirring at a constant speed, and reacting for 6 h. Stopping the reaction, pouring out while the reaction is hot, and crystallizing for 3d at room temperature. The solid particles are washed to neutrality and dried. Burning the mixture for 6 hours at 550 ℃ in a muffle furnace to remove hexadecyl trimethyl ammonium bromide to obtain MCM-41;
(2) weighing 0.3mmol of chromium sulfate hexahydrate solid in a three-necked bottle, adding 10mL of ultrapure water to fully dissolve the chromium sulfate hexahydrate solid, weighing 80-100mL of methanol, adding the methanol into the three-necked bottle, uniformly mixing, dropwise adding 2mL of N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, reacting for 1-2h, then adding 1g of MCM-41 obtained in the step (1), condensing and refluxing at 80 ℃ for 20h, then adding 1.44mL of epoxy chloropropane, continuing to react for 2-4h, cooling, carrying out suction filtration, and washing for 2-3 times by using absolute ethyl alcohol;
(3) finally, 2mol/L hydrochloric acid is added in the step (2) to elute for 2-4h at normal temperature, then the solution is washed to be neutral by deionized water, and the solution is dried at 80 ℃ to obtain a mesoporous molecular sieve MCM-41 surface Cr (III) ion imprinting adsorption material (MCM-41-IIP 3);
comparative example 3:
the rest of the preparation steps are the same as those of the example 3, except that chromium sulfate hexahydrate is not added in the step (2), and the MCM-41 molecular sieve non-imprinted adsorption material (MCM-41-NIP3) is prepared.
Adsorption experiment:
0.01g of adsorbent was weighed and added to 20mL of 50mg/L ionic solution (Cr (III), Cl, respectively)-、NO3 -、SO4 2-、HPO4 2-) The resulting mixture was adsorbed at 25 ℃ for 2 hours, filtered through a 0.45-. mu.m filter membrane, and the ion concentration of the filtrate was measured. According to the change of the ion concentration before and after adsorption, the ion removal rate was calculated as follows:
in the formula: c0: pre-adsorption ion concentration (mg/L); ce: ion concentration (mg/L) after adsorption equilibration.
The samples obtained in examples 1 to 3 and comparative examples 1 to 3 were subjected to the above adsorption test, respectively, and the results are shown in the table:
from the above table, the maximum removal rate of the mesoporous molecular sieve MCM-41 surface Cr (iii) ion imprinted adsorbent material prepared in the embodiment of the present invention to Cr (iii) ions is 97.21%, which is significantly higher than the removal rate of the non-imprinted adsorbent material to Cr (iii) ions and the removal rate of the imprinted adsorbent material to other ions, and can be used for specific identification and selective removal of Cr (iii) ions.
Claims (1)
1. A method for preparing a Cr (III) ion imprinted material based on the surface of an MCM-41 molecular sieve is characterized by comprising the following specific steps:
(1) preparation of MCM-41: weighing 1.2g of hexadecyl trimethyl ammonium bromide into a three-neck flask, simultaneously weighing 90mL of ammonia water and 130mL of distilled water, adding the ammonia water and the distilled water into the three-neck flask together, stirring at 60 ℃ until the hexadecyl trimethyl ammonium bromide is completely dissolved, slowly dropwise adding 5mL of ethyl orthosilicate under vigorous stirring, stirring at a constant speed, reacting for 6 hours, stopping the reaction, pouring out while the reaction is hot, crystallizing for 3 days at room temperature, washing the solid particles to be neutral, drying, and burning for 6 hours at 550 ℃ in a muffle furnace to remove the hexadecyl trimethyl ammonium bromide, thereby obtaining MCM-41;
(2) weighing 0.2-0.3mmol of chromium sulfate hexahydrate solid in a three-necked bottle, adding 10mL of ultrapure water to fully dissolve the chromium sulfate hexahydrate solid, weighing 80-100mL of absolute ethanol, adding the absolute ethanol into the three-necked bottle, uniformly mixing, dropwise adding 2mL of N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, reacting for 1-2h, then adding 1g of MCM-41 obtained in the step (1), condensing and refluxing at 60-80 ℃ for 20h, then adding 1.44mL of epoxy chloropropane, continuing to react for 2-4h, cooling, carrying out suction filtration, and washing for 2-3 times by using the absolute ethanol;
(3) and (3) finally, adding 2mol/L hydrochloric acid in the step (2) to elute for 2-4h at normal temperature, washing with deionized water to be neutral, and drying at 80 ℃ to obtain the Cr (III) ion imprinting material based on the surface of the MCM-41 molecular sieve.
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CN111729659A (en) * | 2020-07-23 | 2020-10-02 | 桂林理工大学 | Preparation method of MCM-41 molecular sieve surface-based Cr (VI) ion imprinted material |
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