CN112175128A - Preparation method of acrylamide crosslinked acrylic acid and montmorillonite hydrogel - Google Patents
Preparation method of acrylamide crosslinked acrylic acid and montmorillonite hydrogel Download PDFInfo
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- CN112175128A CN112175128A CN201910598007.0A CN201910598007A CN112175128A CN 112175128 A CN112175128 A CN 112175128A CN 201910598007 A CN201910598007 A CN 201910598007A CN 112175128 A CN112175128 A CN 112175128A
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- acrylic acid
- montmorillonite
- acrylamide
- hydrogel
- crosslinked acrylic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/04—Polymerisation in solution
- C08F2/10—Aqueous solvent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Polymerisation Methods In General (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention relates to a preparation method of acrylamide crosslinked acrylic acid and montmorillonite hydrogel, which comprises the following raw materials: (ii) acrylamide; montmorillonite; acrylic acid; sodium hydroxide; n, N' methylenebisacrylamide; ammonium persulfate; sodium bisulfite. The invention firstly mixes the main raw materials of acrylamide, montmorillonite, acrylic acid and sodium hydroxide uniformly in a constant temperature water bath kettle. Then in nitrogen atmosphere, adding initiator to make acrylamide hydroxyl produce free radical, self-polymerizing or polymerizing with acrylic acid to form high polymer, then polymerizing montmorillonite on the basis of said high polymer, and making acrylamide cross-linking acrylic acid and montmorillonite hydrogel by means of cross-linking action of cross-linking agent. By controlling the reaction time, the temperature, the addition amount of the montmorillonite and other factors, the acrylamide crosslinked acrylic acid and montmorillonite hydrogel with better performance is prepared.
Description
Technical Field
The invention relates to a preparation method of acrylamide crosslinked acrylic acid and montmorillonite hydrogel.
Technical Field
The hydrogel can remove heavy metal ions in wastewater through the actions of electrostatic attraction, ion exchange, coordination chelation, physical adsorption and the like due to the unique three-dimensional network structure and a large number of active groups capable of forming salts with the heavy metal ions in the structure. The hydrogel material also has better reusability, belongs to renewable energy sources, can still show better adsorbability to heavy metal ions after desorption for many times, has wide raw material sources and lower cost, is simple and easy to control, and can be prepared by a chemical crosslinking method by adding an initiator and a crosslinking agent or a physical crosslinking method. Therefore, in recent years, it has become a research focus of broad scholars.
Montmorillonite is the main mineral component of bentonite ore, and is a clay-like mineral formed by stacking nanometer-thickness silicate sheets with negative electricity on the surface by means of the electrostatic action between the sheets, and the unit cell in the crystal structure of the clay-like mineral is formed by sandwiching a layer of aluminum oxygen octahedron between two layers of silicon oxygen tetrahedron. Montmorillonite has unique one-dimensional layered nano structure and cation exchange property, so that montmorillonite has strong adsorption capacity and cation exchange performance.
Inorganic material montmorillonite is added into hydrogel as an adsorbent for application of wastewater treatment and heavy metal ion adsorption, so that hydrogel with better mechanical property can be obtained, and the defect that the montmorillonite is difficult to recover is overcome. Therefore, in recent years, researchers pay attention to the application of inorganic material reinforced hydrogel materials to heavy metal ions in wastewater. The research on the preparation of acrylamide crosslinked acrylic acid and montmorillonite hydrogel by using acrylamide, acrylic acid and montmorillonite as raw materials, N' -methylene bisacrylamide as a crosslinking agent and ammonium persulfate and sodium bisulfite as an initiator through an aqueous solution polymerization method has not been reported.
Disclosure of Invention
The invention aims to prepare acrylamide crosslinked acrylic acid and montmorillonite hydrogel with better performance by taking inorganic material montmorillonite as an additive, which is used for removing heavy metal ions in wastewater.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the acrylamide crosslinked acrylic acid and montmorillonite hydrogel mainly comprises the following steps:
the first step is as follows: acrylic acid was mixed well with sodium hydroxide, which was required to neutralize 80% of the acrylic acid. To obtain a uniform mixed solution.
The second step is that: and adding montmorillonite into the uniform mixed solution obtained in the first step under the condition of stirring, and continuously stirring until the mixture is uniform. And (3) adding prepared acrylamide after reaching a uniform state, adding initiators of ammonium persulfate and sodium bisulfite after 5 minutes, introducing nitrogen into the device, and adding a crosslinking agent of N, N' -methylene bisacrylamide after 10 minutes. Reacting for 20 minutes to obtain the acrylamide crosslinked acrylic acid and montmorillonite hydrogel.
The third step: taking out the prepared acrylamide crosslinked acrylic acid and montmorillonite hydrogel, respectively washing with absolute ethyl alcohol and deionized water, and performing suction filtration. So as to achieve the purpose of washing away unreacted monomers. Finally, the acrylamide crosslinked acrylic acid and montmorillonite hydrogel is prepared.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, acrylamide, acrylic acid and montmorillonite are subjected to aqueous solution polymerization in an aqueous solution through an initiator and a cross-linking agent, the reaction is completed in a constant-temperature water bath kettle and in a nitrogen atmosphere, and the adopted raw materials are cheap and easy to obtain, so that the acrylamide cross-linked acrylic acid and montmorillonite hydrogel with good performance can be obtained.
Detailed Description
The present invention is described in further detail below with reference to examples, but the embodiments of the present invention are not limited thereto. In the following examples of embodiments; the materials and methods mentioned in the examples are those commonly used in the art unless otherwise specified.
Example 1
Uniformly mixing acrylic acid and sodium hydroxide, wherein the sodium hydroxide is required to neutralize 80% of the acrylic acid to obtain a uniform mixed solution, adding acrylamide under the condition of stirring, adding initiators of ammonium persulfate and sodium bisulfite after 5 minutes, introducing nitrogen into the device, and adding a crosslinking agent of N, N' -methylene-bisacrylamide after 10 minutes. Reacting for 20 minutes to obtain the acrylamide crosslinked acrylic acid hydrogel. And taking out the prepared acrylamide crosslinked acrylic acid hydrogel, respectively washing with absolute ethyl alcohol and deionized water, and performing suction filtration. So as to achieve the purpose of washing away unreacted monomers. Finally, an acrylamide crosslinked acrylic acid hydrogel was prepared.
Example 2
Mixing acrylic acid and sodium hydroxide uniformly, requiring the sodium hydroxide to neutralize 80% of the acrylic acid to obtain a uniform mixed solution, adding 2% of montmorillonite under the condition of stirring, and continuing to stir until the mixture is uniform. And (3) adding prepared acrylamide after reaching a uniform state, adding initiators of ammonium persulfate and sodium bisulfite after 5 minutes, introducing nitrogen into the device, and adding a crosslinking agent of N, N' -methylene bisacrylamide after 10 minutes. Reacting for 20 minutes to obtain the acrylamide crosslinked acrylic acid and montmorillonite hydrogel. Taking out the prepared acrylamide crosslinked acrylic acid and montmorillonite hydrogel, respectively washing with absolute ethyl alcohol and deionized water, and performing suction filtration. So as to achieve the purpose of washing away unreacted monomers. Finally, the acrylamide crosslinked acrylic acid and montmorillonite hydrogel is prepared.
Example 3
Mixing acrylic acid and sodium hydroxide uniformly, requiring the sodium hydroxide to neutralize 80% of the acrylic acid to obtain a uniform mixed solution, adding 4% of montmorillonite under the condition of stirring, and continuing to stir until the mixture is uniform. And (3) adding prepared acrylamide after reaching a uniform state, adding initiators of ammonium persulfate and sodium bisulfite after 5 minutes, introducing nitrogen into the device, and adding a crosslinking agent of N, N' -methylene bisacrylamide after 10 minutes. Reacting for 20 minutes to obtain the acrylamide crosslinked acrylic acid and montmorillonite hydrogel. Taking out the prepared acrylamide crosslinked acrylic acid and montmorillonite hydrogel, respectively washing with absolute ethyl alcohol and deionized water, and performing suction filtration. So as to achieve the purpose of washing away unreacted monomers. Finally, the acrylamide crosslinked acrylic acid and montmorillonite hydrogel is prepared.
Example 4
Mixing acrylic acid and sodium hydroxide uniformly, requiring the sodium hydroxide to neutralize 80% of the acrylic acid to obtain a uniform mixed solution, adding 6% of montmorillonite under the condition of stirring, and continuing to stir until the mixture is uniform. And (3) adding prepared acrylamide after reaching a uniform state, adding initiators of ammonium persulfate and sodium bisulfite after 5 minutes, introducing nitrogen into the device, and adding a crosslinking agent of N, N' -methylene bisacrylamide after 10 minutes. Reacting for 20 minutes to obtain the acrylamide crosslinked acrylic acid and montmorillonite hydrogel. Taking out the prepared acrylamide crosslinked acrylic acid and montmorillonite hydrogel, respectively washing with absolute ethyl alcohol and deionized water, and performing suction filtration. So as to achieve the purpose of washing away unreacted monomers. Finally, the acrylamide crosslinked acrylic acid and montmorillonite hydrogel is prepared.
Claims (2)
1. A preparation method of acrylamide crosslinked acrylic acid and montmorillonite hydrogel is characterized in that the acrylamide crosslinked acrylic acid and montmorillonite hydrogel is composed of the following raw materials: (ii) acrylamide; montmorillonite; acrylic acid; sodium hydroxide; n, N' methylenebisacrylamide; ammonium persulfate; sodium bisulfite. The preparation method of the acrylamide crosslinked acrylic acid and montmorillonite hydrogel comprises the step of preparing the acrylamide crosslinked acrylic acid and montmorillonite hydrogel by solution polymerization of acrylamide, acrylic acid and montmorillonite by using an initiator and a crosslinking agent under a constant temperature condition.
2. The acrylamide crosslinked acrylic acid and montmorillonite hydrogel as claimed in claim 1, wherein the preparation method of the acrylamide crosslinked acrylic acid and montmorillonite hydrogel comprises the following main implementation steps:
the first step is as follows: acrylic acid was mixed well with sodium hydroxide, which was required to neutralize 80% of the acrylic acid. To obtain a uniform mixed solution.
The second step is that: and adding montmorillonite into the uniform mixed solution obtained in the first step under the condition of stirring, and continuously stirring until the mixture is uniform. And (3) adding prepared acrylamide after reaching a uniform state, adding initiators of ammonium persulfate and sodium bisulfite after 5 minutes, introducing nitrogen into the device, and adding a crosslinking agent of N, N' -methylene bisacrylamide after 10 minutes. Reacting for 20 minutes to obtain the acrylamide crosslinked acrylic acid and montmorillonite hydrogel.
The third step: taking out the prepared acrylamide crosslinked acrylic acid and montmorillonite hydrogel, respectively washing with absolute ethyl alcohol and deionized water, and performing suction filtration. So as to achieve the purpose of washing away unreacted monomers. Finally, the acrylamide crosslinked acrylic acid and montmorillonite hydrogel is prepared.
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| CN201910598007.0A CN112175128A (en) | 2019-07-02 | 2019-07-02 | Preparation method of acrylamide crosslinked acrylic acid and montmorillonite hydrogel |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112898925A (en) * | 2021-01-25 | 2021-06-04 | 义乌市鹏之友新材料研究所有限公司 | Adhesive and preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112898925A (en) * | 2021-01-25 | 2021-06-04 | 义乌市鹏之友新材料研究所有限公司 | Adhesive and preparation method and application thereof |
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Application publication date: 20210105 |
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