CN114230719B - Double-crosslinking cellulose-based hydrogel prepared by cold plasma and preparation method and application thereof - Google Patents

Double-crosslinking cellulose-based hydrogel prepared by cold plasma and preparation method and application thereof Download PDF

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CN114230719B
CN114230719B CN202111504454.9A CN202111504454A CN114230719B CN 114230719 B CN114230719 B CN 114230719B CN 202111504454 A CN202111504454 A CN 202111504454A CN 114230719 B CN114230719 B CN 114230719B
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CN114230719A (en
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成军虎
韩卓芮
孙大文
马骥
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South China University of Technology SCUT
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    • 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
    • C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
    • C08F251/02—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof on to cellulose or derivatives thereof
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08F2/00—Processes of polymerisation
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    • C08F2/52—Polymerisation initiated by wave energy or particle radiation by electric discharge, e.g. voltolisation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • 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 double-crosslinking cellulose-based hydrogel prepared by using cold plasma and a preparation method and application thereof, belonging to the field of cellulose-based hydrogels. According to the invention, acrylic Acid (AA) and 2-acrylamide-2-methylpropanesulfonic Acid (AMPS) are added into a cellulose solution, and after cold plasma treatment, the mixture is stirred and mixed uniformly, and then the mixture is stood, washed and dried to obtain the double-crosslinked cellulose hydrogel. The cellulose solution is obtained by precooling a NaOH/urea system, adding dried pineapple peel residue cellulose, stirring and dispersing until the cellulose is completely dissolved, and centrifuging. According to the invention, the pineapple peel residue cellulose is used as a raw material, the cold plasma technology is utilized to initiate and prepare the double-crosslinking cellulose-based hydrogel with good mechanical properties, the use of chemical initiators is reduced, and the preparation method is green and environment-friendly. And a large amount of carboxyl is introduced into the surface of the hydrogel, so that heavy metal ions in the sewage can be efficiently and quickly removed, and the dual purposes of treating wastes with processes of wastes against one another are achieved.

Description

Double-crosslinking cellulose-based hydrogel prepared by cold plasma and preparation method and application thereof
Technical Field
The invention belongs to the field of cellulose-based hydrogel, and particularly relates to double-crosslinking cellulose-based hydrogel prepared by cold plasma and a preparation method and application thereof.
Background
With the increasing of the energy crisis and the increasing of the consciousness of protecting the nature, the development and utilization of natural materials are receiving more and more attention. The natural material is abundant and renewable, and has great utilization potential. Cellulose is widely used as one of the most abundant biomass resources in the world due to its biocompatibility and biodegradability. However, the polyhydroxy structure of cellulose results in a great deal of hydrogen bonds being formed very easily between and within molecules, and shows a great cohesive force, making cellulose difficult to be dissolved in water and most common organic solvents, and thus difficult to be directly utilized. At present, the recovery rate of cellulose is very low, only about 1%, and most of cellulose is discarded, thereby causing resource waste. Thus, cellulose is modified to improve its properties, making it suitable for a wider range of industrial applications.
The hydrogel is a polymer cross-linked network which is formed by hydrophilic polymers and filled with liquid media, contains one or more functional groups, and can adsorb metal ions through ion exchange and complexation. The preparation method of the hydrogel is various, and the preparation method can be divided into physical crosslinking preparation and chemical crosslinking preparation according to different crosslinking effects formed by a crosslinking network structure. The preparation process of the physically crosslinked hydrogel comprises the following steps: through physical actions such as stirring, heating, freezing, irradiating, ultrasonic wave, high pressure and the like, the hydrogel is formed through electrostatic action, ionic interaction, hydrogen bond and chain winding and crosslinking. Physical gels avoid the use of cross-linking agents and exhibit reversibility to external stimuli (temperature, pH, light, etc.). However, physical gel has the disadvantages of poor mechanical properties, long gel forming time, reversible force between molecules of the physically crosslinked cellulose gel, unstable properties, easy damage of the internal structure by external conditions, and no permanence. Therefore, chemical crosslinking assistance is required. The hydrogel prepared by chemical crosslinking is mainly formed into a high molecular polymer with a three-dimensional network structure through chemical reaction and chemical bond. Most of them are carried out by free radical polymerization, i.e. various initiation systems are adopted to induce cellulose to generate macromolecular chain free radicals, and then the macromolecular chain free radicals are grafted and copolymerized with monomers. At present, chemical initiation, ultraviolet initiation and high-energy particle radiation initiation are mainly adopted in hydrogel preparation initiation technologies, and most of hydrogels prepared by the initiation technologies have the problems of unreacted monomers, initiator residues, high energy consumption and the like.
Patent CN201910456859.6 discloses a preparation method of a cellulose-based hydrogel adsorbent for heavy metal wastewater treatment, which is characterized in that cotton yarn cellulose is dissolved, then the cotton yarn cellulose is graft-copolymerized with monomer Acrylic Acid (AA) under the action of initiator Ammonium Persulfate (APS), a gel-like polymer is prepared under the action of cross-linking agent N, N-Methylene Bisacrylamide (MBA), a mixed modified solution of dimethyl sulfoxide, epichlorohydrin and triethylene tetramine is placed into the gel-like polymer for soaking and heating, and after the reaction is finished, alcohol and water are repeatedly used for cleaning to obtain a cellulose hydrogel finished product. The modified hydrogel prepared by the method has a large amount of amino groups introduced on the surface, has strong heavy metal adsorption capacity, but the method needs to use a large amount of cellulose dissolving solution, initiator and modified solution, and the chemical reagents are toxic, pollute the environment, are expensive and are difficult to recover. In addition, the gel polymer needs to be repeatedly cleaned after being soaked in the modification solution to obtain a finished product, the process is complex, and a certain energy consumption problem exists in the actual production process.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide the double-crosslinking cellulose-based hydrogel prepared by the cold plasma and the preparation method and application thereof.
The purpose of the invention is realized by the following technical scheme.
A method for preparing a dual-crosslinked cellulose-based hydrogel by using cold plasma comprises the following steps:
and (AA) and 2-acrylamide-2-methylpropanesulfonic Acid (AMPS) are added into the cellulose solution, and the mixture is stirred and mixed uniformly after being subjected to cold plasma treatment, and is kept stand, washed and dried to obtain the double-crosslinking cellulose-based hydrogel.
Preferably, the voltage of the cold plasma treatment is 100-150kV, the frequency is 50-70Hz, the power is 45-60kW, and the treatment time is 15-60min.
Preferably, the voltage of the cold plasma treatment is 150kV, the frequency is 50Hz, the power is 45kW, and the treatment time is 60min.
Preferably, the preparation of the cellulose solution comprises the following steps:
precooling a NaOH/urea system, adding dried pineapple peel residue cellulose, stirring and dispersing until the cellulose is completely dissolved, and centrifuging to obtain a cellulose solution.
Preferably, the mass ratio of NaOH, urea and water in the NaOH/urea system is 7; the pre-cooling temperature is-12 to-8 ℃, and the time is 45-60min.
Preferably, the addition amount of the pineapple peel residue cellulose is 2.5-3.0% of the mass of a NaOH/urea system.
Preferably, the speed of the centrifugation is 5000r/min, and the time is 5min.
Preferably, the addition amount of the acrylic acid is 2-3 times of the dry basis weight of the pineapple peel residue cellulose; the addition amount of the 2-acrylamide-2-methylpropanesulfonic acid is 0.2-0.3 time of the dry basis weight of the pineapple peel residue cellulose.
Preferably, the standing time is 18-24h.
Preferably, the washing is water washing or acetone washing.
Preferably, the drying is vacuum drying.
A dual cross-linked cellulose-based hydrogel prepared by the method of any one of the above.
Tensile Property test was performed at room temperature using a Universal mechanical testing machine Shimadzu CMT4204, and the tensile Property test was performed at 5 mm. Min -1 The speed of (3) stretches the hydrogel sample. The hydrogel fracture toughness value is obtained by calculating the curve area through integration according to the stress-strain curve before the tensile fracture (stress peak) of the sample. The tensile strength of the conventional cellulose hydrogel was measured to be about 0.16MPa, while the tensile strength of the double cross-linked cellulose-based hydrogel prepared by any of the methods described above was 1.33-2.15MPa.
The application of the double-crosslinked cellulose-based hydrogel in removing heavy metal ions comprises the following steps:
and putting the double-crosslinked cellulose-based hydrogel into a heavy metal ion solution, and stirring and adsorbing.
Preferably, the heavy metal ion solution contains Zn 2+ 、Cd 2+ And Cr 3+ The concentration of heavy metal ions in the mixed solution is 600-1000mg/L, and the pH value is 6.0-7.0.
Preferably, the adsorption time is 45-60min, the removal rate of heavy metal ions reaches 56-72%, and is improved by 45-90% compared with the removal rate of heavy metal ions of the traditional cellulose hydrogel.
In the invention, firstly, the pineapple peel residue cellulose is dissolved by an alkali/urea solvent system, then monomer Acrylic Acid (AA) and cross-linking agent 2-acrylamide-2-methylpropanesulfonic Acid (AMPS) are added, cold plasma is treated for a period of time, and then the product can be obtained after standing and refining.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) Hydroxyl free radicals generated in the discharging process of Cold Plasma (CP) are used as an initiator, and the cellulose hydrogel with a chemical crosslinking network structure is prepared through free radical polymerization reaction, so that the use of chemical reagents is reduced, the method is green and environment-friendly, and the energy consumption is reduced.
(2) H generated by dissolving nitrogen oxide in plasma discharge process + The cellulose chains are exposed due to the removal of an alkali-urea coating system, a physical crosslinking network structure is formed under the action of a strong hydrogen bond and a highly ordered network structure in the cellulose, the double crosslinking cellulose hydrogel with strong stretching and high toughness is obtained, and the softness and fragility of the traditional cellulose hydrogel material are improved.
(3) After the cold plasma treatment, the oxygen-containing functional groups of the cellulose are increased, wherein the carboxyl groups can adsorb heavy metal ions in the solution through strong electrostatic attraction. Therefore, the invention utilizes the cold plasma technology to modify the cellulose hydrogel while preparing the cellulose hydrogel, and the quantity of carboxyl in the obtained cellulose hydrogel is increased, thereby achieving better heavy metal ion adsorption effect.
(4) The cold plasma discharge has an etching effect on the cellulose surface of the pineapple peel residue, and more pore channels are formed on the smooth cellulose surface, so that the adsorption and diffusion of heavy metal ions are facilitated, the adsorption rate of hydrogel is improved, the heavy metal ions in the wastewater can be efficiently and quickly removed, the time and the cost are saved, and the large-scale production is facilitated.
(5) The hydrogel is applied to the adsorption of heavy metal ions, the pollution load of wastewater is reduced, and the hydrogel serving as a biological adsorbent can be recycled and degraded, so that the wastewater treatment cost is reduced.
(6) The typical tropical fruit and vegetable processing waste pineapple peel is used as a raw material, so that the utilization value of the pineapple peel residue cellulose is improved, the application range of the pineapple peel residue cellulose is expanded, the problem of heavy metal ion pollution of a water body is solved, and the dual purposes of treating wastes with processes of wastes against one another are achieved.
Drawings
FIG. 1 is a schematic diagram of a process for preparing a dual cross-linked cellulose hydrogel according to the present invention; where the bars represent cellulose chains, the diamonds represent monomers, the triangles represent cross-linking agents, and the dots represent base/urea solutions.
FIG. 2 is a flow chart of the present invention for preparing a double cross-linked cellulose-based hydrogel.
FIG. 3 is a graph showing the removal rate of heavy metal ions from the hydrogels obtained in examples 1 to 4 as they are according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
The schematic diagram and the flow chart of the preparation of the double-crosslinking cellulose hydrogel are shown in the figures 1 and 2.
Example 1
The method for preparing the double-crosslinked cellulose-based hydrogel based on the cold plasma and the application thereof in the embodiment are specifically as follows:
weighing 7g of NaOH and 12g of urea, dissolving in 81g of deionized water, and freezing at-12 ℃ for 1h to obtain a NaOH/urea system. Weighing 2g of dried pineapple peel residue cellulose, placing the dried pineapple peel residue cellulose in a NaOH/urea system, stirring and dispersing until the cellulose is completely dissolved, and centrifuging at the rotating speed of 5000r/min for 5min to obtain a cellulose solution. Weighing 6g of Acrylic Acid (AA) and 0.6g of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), adding the mixture into a cellulose solution, carrying out cold plasma treatment (the voltage is 100kV, the frequency is controlled to be 50Hz, and the power is controlled to be 45 kW) for 15min, stirring and mixing uniformly, standing at room temperature for 24h, washing a product with water and acetone, and drying in vacuum to constant weight to obtain the double-crosslinked cellulose hydrogel. Putting the prepared cellulose-based hydrogel into Zn with the concentration of 800mg/L and the pH value of 6.5 2+ ，Cd 2+ And Cr 3+ Mixing with heavy metal ion solution, stirring and adsorbing for 60min. Through measurement, the tensile strength of the double-crosslinked cellulose-based hydrogel of the embodiment is 1.33MPa, and the removal rate of heavy metal ions is 56%, which is higher than that of the conventional cellulose hydrogelThe removal rate of the glue to heavy metal ions increased by 47% (see fig. 3, "as is" in fig. 3 refers to a conventional cellulose hydrogel).
Example 2
Weighing 7g of NaOH and 12g of urea, dissolving in 81g of deionized water, and freezing at-12 ℃ for 1h to obtain a NaOH/urea system. Weighing 2g of dried pineapple peel residue cellulose, placing the dried pineapple peel residue cellulose in a NaOH/urea system, stirring and dispersing until the cellulose is completely dissolved, and centrifuging at the rotating speed of 5000r/min for 5min to obtain a cellulose solution. Weighing 6g of Acrylic Acid (AA) and 0.6g of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), adding the mixture into a cellulose solution, carrying out cold plasma treatment (the voltage is 120kV, the frequency is controlled to be 50Hz, and the power is controlled to be 45 kW), wherein the treatment time is 30min, stirring and mixing the mixture uniformly, standing the mixture at room temperature for 24h, washing a product by water and acetone, and drying the product in vacuum to constant weight to obtain the double-crosslinked cellulose hydrogel. Putting the prepared cellulose-based hydrogel into Zn with the concentration of 600mg/L and the pH value of 6.5 2+ ，Cd 2+ And Cr 3+ Mixing with heavy metal ion solution, stirring and adsorbing for 60min. It was determined that the tensile strength of the double-crosslinked cellulose-based hydrogel of this example was 1.67MPa, and the removal rate of heavy metal ions was 61%, which was improved by 61% compared to the removal rate of heavy metal ions of the conventional cellulose hydrogel (see FIG. 3).
Example 3
Weighing 7g of NaOH and 12g of urea, dissolving in 81g of deionized water, and freezing at-12 ℃ for 1h to obtain a NaOH/urea system. Weighing 2g of dried pineapple peel residue cellulose, placing the dried pineapple peel residue cellulose in a NaOH/urea system, stirring and dispersing until the cellulose is completely dissolved, and centrifuging at the rotating speed of 5000r/min for 5min to obtain a cellulose solution. Weighing 6g of Acrylic Acid (AA) and 0.6g of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS) and adding the mixture into a cellulose solution, then carrying out cold plasma treatment (the voltage is 150kV, the frequency is controlled to be 50Hz, and the power is controlled to be 45 kW), wherein the treatment time is 45min, stirring and mixing uniformly, standing at room temperature for 24h, washing a product with water and acetone, and drying in vacuum to constant weight to obtain the dual-crosslinked cellulose hydrogel. Putting the prepared cellulose-based hydrogel into Zn with the concentration of 800mg/L and the pH value of 6 2+ ，Cd 2+ And Cr 3+ Mixing with heavy metal ion solution, stirring and adsorbing for 60min. By measurement, this exampleThe tensile strength of the example double-crosslinked cellulose-based hydrogel was 1.98MPa, and the removal rate of heavy metal ions was 67%, which was 76% higher than that of the conventional cellulose hydrogel (see fig. 3).
Example 4
Weighing 7g of NaOH and 12g of urea, dissolving in 81g of deionized water, and freezing at-12 ℃ for 1h to obtain a NaOH/urea system. Weighing 2g of dried pineapple peel residue cellulose, placing the dried pineapple peel residue cellulose in a NaOH/urea system, stirring and dispersing until the cellulose is completely dissolved, and centrifuging at the rotating speed of 5000r/min for 5min to obtain a cellulose solution. Weighing 6g of Acrylic Acid (AA) and 0.6g of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS) and adding the mixture into a cellulose solution, then carrying out cold plasma treatment (the voltage is 150kV, the frequency is controlled to be 50Hz, and the power is controlled to be 45 kW), wherein the treatment time is 60min, stirring and mixing uniformly, standing at room temperature for 24h, washing a product with water and acetone, and drying in vacuum to constant weight to obtain the dual-crosslinked cellulose hydrogel. Putting the prepared cellulose-based hydrogel into Zn with the concentration of 800mg/L and the pH value of 5.5 2+ ，Cd 2+ And Cr 3+ Mixing with heavy metal ion solution, stirring and adsorbing for 60min. Through measurement, the tensile strength of the double-crosslinked cellulose-based hydrogel of the present example is 2.15MPa, and the removal rate of heavy metal ions is 72%, which is 89% higher than that of the conventional cellulose hydrogel (see fig. 3).
Comparative example 1
Weighing 7g of NaOH and 12g of urea, dissolving in 81g of deionized water, and freezing at-12 ℃ for 1h to obtain a NaOH/urea system. Weighing 2g of dried pineapple peel residue cellulose, placing the dried pineapple peel residue cellulose in a NaOH/urea system, stirring and dispersing until the cellulose is completely dissolved, and centrifuging at the rotating speed of 5000r/min for 5min to obtain a cellulose solution. 3g of Ammonium Persulfate (APS), 6g of Acrylic Acid (AA) and 0.6g of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS) are weighed and added into a cellulose solution, and after the reaction is finished, the cellulose hydrogel finished product is obtained after repeated cleaning by using alcohol and water. Putting the prepared cellulose-based hydrogel into Zn with the concentration of 800mg/L and the pH value of 5.5 2+ ，Cd 2+ And Cr 3+ Mixing with heavy metal ion solution, stirring and adsorbing for 60min. The tensile strength was measured to be 0.16MPa, and the removal rate of heavy metal ions was 38%.
Comparative example 2
Weighing 7g of NaOH and 12g of urea, dissolving in 81g of deionized water, and freezing at-12 ℃ for 1h to obtain a NaOH/urea system. Weighing 2g of dried pineapple peel residue cellulose, placing the dried pineapple peel residue cellulose in a NaOH/urea system, stirring and dispersing until the cellulose is completely dissolved, and centrifuging at the rotating speed of 5000r/min for 5min to obtain a cellulose solution. 6g of Ammonium Persulfate (APS), 12g of Acrylic Acid (AA) and 1.2g of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS) are weighed and added into a cellulose solution, and after the reaction is finished, alcohol and water are used for repeatedly cleaning to obtain a cellulose hydrogel finished product. Putting the prepared cellulose-based hydrogel into Zn with the concentration of 800mg/L and the pH value of 5.5 2+ ，Cd 2+ And Cr 3+ Mixing with heavy metal ion solution, stirring and adsorbing for 60min. The tensile strength was measured to be 0.23MPa, and the removal rate of heavy metal ions was 42%.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such modifications are intended to be included in the scope of the present invention.

Claims (9)

1. A method for preparing a dual-crosslinking cellulose-based hydrogel by using cold plasma is characterized by comprising the following steps:
adding acrylic acid and 2-acrylamide-2-methylpropanesulfonic acid into a cellulose solution, carrying out cold plasma treatment, stirring and mixing uniformly, standing, washing and drying to obtain the double-crosslinked cellulose-based hydrogel;
the preparation of the cellulose solution comprises the following steps:
precooling a NaOH/urea system, adding dried pineapple peel residue cellulose, stirring and dispersing until the cellulose is completely dissolved, and centrifuging to obtain a cellulose solution.
2. The method according to claim 1, characterized in that the cold plasma treatment is carried out at a voltage of 100-150kV, at a frequency of 50-70Hz, at a power of 45-60kW and for a treatment time of 15-60min.
3. The method according to claim 2, characterized in that the cold plasma treatment is carried out at a voltage of 150kV, a frequency of 50Hz, a power of 45kW and a treatment time of 60min.
4. A process according to any one of claims 1 to 3, characterized in that the mass ratio of NaOH, urea, water in the NaOH/urea system is 7; the pre-cooling temperature is-12 to-8 ℃, and the time is 45-60min.
5. The method according to any one of claims 1 to 3, wherein the pineapple peel residue cellulose is added in an amount of 2.5 to 3.0% by mass of the NaOH/urea system; the addition amount of the acrylic acid is 2-3 times of the dry basis weight of the pineapple peel residue cellulose; the addition amount of the 2-acrylamide-2-methylpropanesulfonic acid is 0.2-0.3 time of the dry basis weight of the pineapple peel residue cellulose.
6. A method according to any one of claims 1 to 3, wherein the time of standing is 18 to 24 hours.
7. A dual cross-linked cellulose-based hydrogel prepared by the method of any one of claims 1-3.
8. Use of the double cross-linked cellulose-based hydrogel according to claim 7 for removing heavy metal ions, comprising the steps of:
and putting the double-crosslinked cellulose-based hydrogel into a heavy metal ion solution, and stirring and adsorbing.
9. The method according to claim 8, wherein the heavy metal ion solution is Zn-containing 2+ 、Cd 2+ And Cr 3 + The concentration of heavy metal ions in the mixed solution is 600-1000mg/L, and the pH value is 6.0-7.0; the adsorption time is 45-60min.
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