CN112934189A - Peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment, and preparation method and application thereof - Google Patents
Peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment, and a preparation method and application thereof. The method comprises the following steps: soaking the powder pretreated by hydrochloric acid in a mixed system of sodium hydroxide, urea and water to obtain a lignocellulose solution; and (3) uniformly mixing the solution with acrylic acid and beta-cyclodextrin according to a ratio, adding a cross-linking agent and an initiator, carrying out cross-linking and polymerization reaction in a water bath, and cleaning after the reaction is finished to obtain the composite hydrogel. The hydrogel adsorbent has the advantages of simple preparation, wide monomer source, low cost and the like, provides a new way for the resource utilization of the peanut shells, and can realize the purpose of treating wastes with processes of wastes against one another; meanwhile, the gel has high water swelling property, so that adsorption sites in a network can be fully exposed, high-efficiency removal of heavy metal ions is realized, and the gel can be applied to treatment of various heavy metal-containing wastewater.
Description
Technical Field
The invention belongs to the technical field of environmental functional materials and water treatment, relates to a composite hydrogel adsorbent, and particularly relates to a peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment, and a preparation method and application thereof.
Background
In recent years, heavy metal pollution has attracted public attention. In order to improve the current situation of heavy metal pollution, various treatment technologies such as ion exchange, chemical precipitation, extraction, filtration, adsorption, etc. have been used to remove toxic heavy metal ions from water. Among them, the adsorption method is considered to be a simple and effective technique because of its advantages such as simple operation and high cost effectiveness. The existing adsorption materials mostly use nano and particle adsorbents as main materials, the adsorption sites on the surfaces of the adsorbents are easy to block and lose adsorption capacity, and the small particle size causes difficult separation, thereby greatly limiting the practical application of the adsorbents. The hydrogel material has simple preparation, adjustable mechanical property and wide monomer source, and is widely used in the fields of biomedicine, food industry, soft machine machinery, heavy metal separation and the like. However, the poor mechanical properties of single-monomer hydrogel materials limit their wide application.
The agricultural and forestry wastes have the advantages of no toxicity, no harm, reproducibility, sustainability, biodegradability and the like. Meanwhile, lignocellulose in the agricultural and forestry waste contains various surface functional groups such as hydroxyl, carboxyl, sulfydryl, nitrogen, phosphorus, sulfur and the like, and has strong adsorption capacity, so that the preparation of the adsorption material by utilizing the agricultural and forestry waste attracts wide attention. Peanut shells are common agricultural wastes in China, and have the advantages of wide sources, high yield and high lignocellulose content. However, the adsorbent obtained by only using peanut shells or simply modifying the peanut shells has limited adsorption capacity to heavy metal ions and long adsorption time, so that how to improve the adsorption performance of the peanut shell adsorbent to heavy metals is still needed to be researched.
The beta-cyclodextrin has a hollow round table structure, the outer side of the beta-cyclodextrin is hydrophilic, the inner side of the beta-cyclodextrin is hydrophobic, and the special structure and property enable the beta-cyclodextrin and the polymer thereof to be widely applied to the fields of material separation and adsorption, environmental protection and the like.
Chinese patent CN110975832A discloses a straw-based hydrogel adsorbent for efficiently removing heavy metal ions and a preparation method thereof. The method is characterized in that acrylonitrile polymers are grafted on the surfaces of modified straws to prepare acrylonitrile polymer modified straw-based hydrogel which is used for treating heavy metal solution. However, the preparation process needs a plurality of chemical reagents, the preparation is complex, the application cost is increased, and large-scale popularization and application are not facilitated.
Disclosure of Invention
The invention aims to overcome the defects of the adsorption performance and application of an adsorbent in the prior art and the problem that peanut shell waste is difficult to recycle, and provides a peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment, and a preparation method and application thereof.
The preparation method provided by the invention is a preparation method of the peanut shell lignocellulose/polyacrylic acid/beta-cyclodextrin composite hydrogel adsorbent with simple process and high adsorption efficiency.
The preparation method provided by the invention extracts lignocellulose in the peanut shells by selecting a mixed system of urea, sodium hydroxide and water; uniformly mixing the obtained lignocellulose solution with acrylic acid and beta-cyclodextrin, and then selecting a specific cross-linking agent and an initiator to complete gelation by adopting a water bath method. The efficient peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent provided by the invention has the advantages of excellent adsorption performance, better mechanical property, high water swelling performance, simple process and easiness in operation, and can be applied to the actual industrial treatment process.
The invention also aims to provide a preparation method of the peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment.
The invention further aims to provide application of the peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment in a water body.
The purpose of the invention is realized by at least one of the following technical solutions.
The invention provides a preparation method of a peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment, which comprises the following steps:
(1) cleaning and airing the collected peanut shells, then crushing the peanut shells by using a crusher, and sieving to obtain peanut shell powder;
(2) soaking the peanut shell powder in the step (1) in a hydrochloric acid solution, stirring, filtering to obtain a precipitate, washing the precipitate to be neutral by using deionized water, and drying to obtain pretreated peanut shell powder;
(3) dissolving sodium hydroxide and urea in water, and uniformly mixing to obtain a mixed solution; adding the pretreated peanut shell powder obtained in the step (2) into the mixed solution (the pretreated peanut shell powder needs to be fully soaked in the mixed solution), stirring, centrifuging and taking supernate to obtain a lignin fiber solution;
(4) adding acrylic acid and a beta-cyclodextrin solution into the lignin fiber solution obtained in the step (3), uniformly mixing, adding ammonium persulfate and N, N-methylene bisacrylamide, and uniformly mixing to obtain a mixed solution;
(5) and (3) heating the mixed solution obtained in the step (4) in a closed container to carry out water bath heating treatment to obtain gel, washing with deionized water, and drying to constant weight to obtain the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for treating heavy metal wastewater.
Further, the size of the sieve holes of the sieve in the step (1) is 60-100 meshes.
Preferably, the size of the sieve of step (1) is 80-100 meshes.
Further, in the step (1), the washing is repeatedly washing with clean water and deionized water.
Further, the concentration of the hydrochloric acid solution in the step (2) is 0.5-1.0 mol/L; the mass volume ratio of the peanut shell powder to the hydrochloric acid solution is 15-25: 1 g/L; the stirring treatment time is 8-16 h.
Further, the mass ratio of the sodium hydroxide, the urea and the water in the step (3) is (5-10): (10-15): (75-85).
Further, the mass ratio of the pretreated peanut shell powder in the step (3) to the mixed solution is (8-15): (80-120); the stirring treatment time is 8-16 h.
Further, the rotation speed of the centrifugation in the step (3) is 8000-10000r/min, and the centrifugation time is 5-15 min.
Further, the mass percentage concentration of the cyclodextrin solution in the step (4) is 1-5%; the volume ratio of the lignin fiber solution to the acrylic acid and cyclodextrin solution is (6-16): (3-8): (3-8); the molar ratio of the acrylic acid, the ammonium persulfate and the N, N-methylene-bisacrylamide in the step (4) is 100: (0.1-0.25): (1-2). The cyclodextrin solution is beta-cyclodextrin solution.
Further, the temperature of the water bath heating treatment is 50-70 ℃, and the time of the water bath heating treatment is 2-4 h; the washing comprises the following steps: soaking the gel in water for 12-24h, taking out, and washing the gel with water again; the drying temperature is 50-60 ℃.
Preferably, the gelation treatment in step (5) may be performed by heating the mixed solution in a water bath to raise the temperature of the mixed solution.
Preferably, the washing of step (5) comprises: and soaking the gel in deionized water and alcohol for 12-24h, taking out, and washing the gel with deionized water again.
The invention provides a peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment, which is prepared by the preparation method.
The composite hydrogel adsorbent is prepared by performing simple free radical polymerization on lignocellulose, acrylic acid and beta-cyclodextrin monomers extracted from peanut shells to obtain the composite hydrogel with a three-dimensional porous net structure.
The invention provides application of a peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment in treating polluted wastewater as a heavy metal adsorbent.
The peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment can be applied to water treatment to remove Pb2+And Cd2+。
The invention uses the lignocellulose extracted from the peanut shells, the beta-cyclodextrin and the acrylic acid as the monomers to synthesize the composite hydrogel, overcomes the defect of a single monomer hydrogel material, can realize the resource utilization of the peanut shells and can also realize the efficient removal of heavy metal ions in a water body.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the preparation method provided by the invention uses the agricultural and forestry waste peanut shells as the raw material, has low cost, can realize the treatment of wastes with processes of wastes against one another, and conforms to the sustainable development strategy.
(2) According to the preparation method provided by the invention, beta-cyclodextrin is used as a monomer, the special structure of the beta-cyclodextrin, which is hydrophilic in the outer cavity and hydrophobic in the inner cavity, has good adsorption performance on heavy metal ions, the water swelling performance of the composite hydrogel material is reduced, and the mechanical performance of the composite hydrogel is enhanced.
(3) The peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for treating heavy metal wastewater provided by the invention is simple in preparation process and low in equipment requirement; the material has good adsorption performance on heavy metal ions, and can effectively remove the heavy metal ions in the wastewater.
Drawings
FIG. 1 is a high-resolution Scanning Electron Microscope (SEM) image of a peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment in example 1 of the present invention;
FIG. 2 is a high-resolution Scanning Electron Microscope (SEM) image of a peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment in example 2 of the present invention;
FIG. 3 shows Cd pairs of peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbents for heavy metal wastewater treatment in embodiments 1, 2, 4, 6 and 7 of the present invention2+The removal effect map of (1).
FIG. 4 is an infrared spectrum (FT-IR) of a peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment in example 1 of the present invention;
FIG. 5 is an X-ray fluorescence diffraction pattern (XRD) of the peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment in example 1 of the present invention;
FIG. 6a is a compression energy diagram of a peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment provided in example 1 of the present invention;
FIG. 6b is a tensile strength diagram of the peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment provided in example 1 of the present invention;
FIG. 7 is a compression resistance force diagram of the peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment provided in example 4 of the invention
FIG. 8 is a tensile strength diagram of a peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment provided in example 8 of the present invention;
fig. 9 is a graph of the adsorption effect of different addition amounts of the peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment on pb (ii) provided in embodiment 1 of the present invention;
FIG. 10a is a graph showing the adsorption kinetics of a peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment on Pb (II) provided in example 1 of the present invention;
fig. 10b is a graph of adsorption kinetics of cd (ii) by the peanut shell lignocellulose/β -cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment provided in embodiment 1 of the present invention;
FIG. 11 shows that the peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment provided in embodiment 1 of the present invention is used for adsorbing Cd at different concentrations2+A graph of adsorption rate and adsorption capacity of (a);
fig. 12a and 12b are force diagrams of compression and tensile resistance, respectively, of a composite hydrogel material synthesized without the addition of beta-cyclodextrin.
Detailed Description
The following examples are presented to further illustrate the practice of the invention, but the practice and protection of the invention is not limited thereto. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
Example 1
A preparation method of a peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment comprises the following steps:
(1) repeatedly cleaning peanut shells with clear water and deionized water, naturally drying, pulverizing with a pulverizer, and sieving (with 80 mesh sieve) to obtain peanut shell powder;
(2) soaking 25g of the peanut shell powder obtained in the step (1) in 1.0L of hydrochloric acid solution (with the concentration of 1mol/L), stirring for 12 hours, filtering to obtain a precipitate, washing the precipitate to be neutral, and drying in an oven at 50 ℃ to obtain pretreated peanut shell powder;
(3) dissolving 7.0g of sodium hydroxide and 12.0g of urea in 81g of water, and uniformly mixing to obtain a mixed solution; adding 9.0g of the pretreated peanut shell powder obtained in the step (2) into the mixed solution, stirring for 12 hours, centrifuging to obtain a supernatant (the centrifugation speed is 8000r/min, and the time is 10min), and obtaining a lignin fiber solution;
(4) adding 5mL of acrylic acid and 5mL of beta-cyclodextrin solution (the concentration is 1 wt%) into 10mL of the lignin fiber solution obtained in the step (3), uniformly mixing, adding 416.0mg of ammonium persulfate and 168.8mg of N, N-methylene-bisacrylamide, and uniformly mixing to obtain a mixed solution;
(5) and (3) transferring the mixed solution obtained in the step (4) into a glass sealed container, heating in a water bath heating mode to carry out gelation treatment (the temperature is 70 ℃ and the time is 3 hours) to obtain gel, soaking and washing the gel in deionized water to remove unreacted substances, wherein the soaking time is 24 hours, and drying the gel in a 50 ℃ oven to obtain the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for treating heavy metal wastewater.
Example 2
A preparation method of a peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment comprises the following steps:
(1) repeatedly cleaning peanut shells with clear water and deionized water, naturally drying, pulverizing with a pulverizer, and sieving (with 80 mesh sieve) to obtain peanut shell powder;
(2) soaking 25g of the peanut shell powder obtained in the step (1) in 1.0L of hydrochloric acid solution (with the concentration of 1mol/L), stirring for 12 hours, filtering to obtain a precipitate, washing the precipitate to be neutral, and drying in an oven at 50 ℃ to obtain pretreated peanut shell powder;
(3) dissolving 7.0g of sodium hydroxide and 12.0g of urea in 81g of water, and uniformly mixing to obtain a mixed solution; adding 9.0g of the pretreated peanut shell powder obtained in the step (2) into the mixed solution, stirring for 12 hours, centrifuging to obtain a supernatant (the centrifugation speed is 8000r/min, and the time is 10min), and obtaining a lignin fiber solution;
(4) adding 5mL of acrylic acid and 5mL of beta-cyclodextrin solution (the concentration is 2 wt%) into 10mL of the lignin fiber solution obtained in the step (3), uniformly mixing, adding 416.0mg of ammonium persulfate and 168.8mg of N, N-methylene-bisacrylamide, and uniformly mixing to obtain a mixed solution;
(5) and (3) transferring the mixed solution obtained in the step (4) into a glass sealed container, heating in a water bath heating mode to carry out gelation treatment (the temperature is 70 ℃ and the time is 3 hours) to obtain gel, soaking and washing the gel in deionized water to remove unreacted substances, wherein the soaking time is 24 hours, and drying the gel in a 50 ℃ oven to obtain the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for treating heavy metal wastewater.
Example 3
A preparation method of a peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment comprises the following steps:
(1) repeatedly cleaning peanut shells with clear water and deionized water, naturally drying, pulverizing with a pulverizer, and sieving (with sieve mesh of 60 meshes) to obtain peanut shell powder;
(2) soaking 25g of the peanut shell powder obtained in the step (1) in 1.0L of hydrochloric acid solution (with the concentration of 1mol/L), stirring for 16h, filtering to obtain a precipitate, washing the precipitate to be neutral, and drying in an oven at 50 ℃ to obtain pretreated peanut shell powder;
(3) dissolving 7.0g of sodium hydroxide and 12.0g of urea in 81g of water, and uniformly mixing to obtain a mixed solution; adding 9.0g of the pretreated peanut shell powder obtained in the step (2) into the mixed solution, stirring for 16h, centrifuging to obtain a supernatant (the centrifugation speed is 8000r/min, and the centrifugation time is 15min) to obtain a lignin fiber solution;
(4) adding 5mL of acrylic acid and 5mL of beta-cyclodextrin solution (the concentration is 2 wt%) into 10mL of the lignin fiber solution obtained in the step (3), uniformly mixing, adding 416.0mg of ammonium persulfate and 168.8mg of N, N-methylene-bisacrylamide, and uniformly mixing to obtain a mixed solution;
(5) and (3) transferring the mixed solution obtained in the step (4) into a glass sealed container, heating in a water bath heating mode to carry out gelation treatment (the temperature is 60 ℃ and the time is 4 hours) to obtain gel, soaking and washing the gel in deionized water to remove unreacted substances, wherein the soaking time is 24 hours, and drying the gel in a 50 ℃ oven to obtain the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for treating heavy metal wastewater.
Example 4
A preparation method of a peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment comprises the following steps:
(1) repeatedly cleaning peanut shells with clear water and deionized water, naturally drying, pulverizing with a pulverizer, and sieving (with 80 mesh sieve) to obtain peanut shell powder;
(2) soaking 25g of the peanut shell powder obtained in the step (1) in 1.0L of hydrochloric acid solution (with the concentration of 1mol/L), stirring for 12 hours, filtering to obtain a precipitate, washing the precipitate to be neutral, and drying in an oven at 50 ℃ to obtain pretreated peanut shell powder;
(3) dissolving 7.0g of sodium hydroxide and 12.0g of urea in 81.0g of water, and uniformly mixing to obtain a mixed solution; adding 9.0g of the pretreated peanut shell powder obtained in the step (2) into the mixed solution, stirring for 12 hours, centrifuging to obtain a supernatant (the centrifugation speed is 8000r/min, and the time is 10min), and obtaining a lignin fiber solution;
(4) adding 5mL of acrylic acid and 5mL of beta-cyclodextrin solution (the concentration is 3 wt%) into 10mL of the lignin fiber solution obtained in the step (3), uniformly mixing, adding 416.0mg of ammonium persulfate and 168.8mg of N, N-methylene-bisacrylamide, and uniformly mixing to obtain a mixed solution;
(5) and (3) transferring the mixed solution obtained in the step (4) into a glass sealed container, heating in a water bath heating mode to carry out gelation treatment (the temperature is 70 ℃ and the time is 3 hours) to obtain gel, soaking and washing the gel in deionized water to remove unreacted substances, wherein the soaking time is 24 hours, and drying the gel in a 50 ℃ oven to obtain the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for treating heavy metal wastewater.
Example 5
A preparation method of a peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment comprises the following steps:
(1) repeatedly cleaning peanut shells with clear water and deionized water, naturally drying, pulverizing with a pulverizer, and sieving (with sieve mesh of 60 meshes) to obtain peanut shell powder;
(2) soaking 25g of the peanut shell powder obtained in the step (1) in 1.0L of hydrochloric acid solution (with the concentration of 1mol/L), stirring for 16h, filtering to obtain a precipitate, washing the precipitate to be neutral, and drying in an oven at 50 ℃ to obtain pretreated peanut shell powder;
(3) dissolving 7.0g of sodium hydroxide and 12.0g of urea in 81.0g of water, and uniformly mixing to obtain a mixed solution; adding 9.0g of the pretreated peanut shell powder obtained in the step (2) into the mixed solution, stirring for 16h, centrifuging to obtain a supernatant (the centrifugation speed is 8000r/min, and the centrifugation time is 15min) to obtain a lignin fiber solution;
(4) adding 5mL of acrylic acid and 5mL of beta-cyclodextrin solution (the concentration is 3 wt%) into 10mL of the lignin fiber solution obtained in the step (3), uniformly mixing, adding 416.0mg of ammonium persulfate and 168.8mg of N, N-methylene-bisacrylamide, and uniformly mixing to obtain a mixed solution;
(5) and (3) transferring the mixed solution obtained in the step (4) into a glass sealed container, heating in a water bath heating mode to carry out gelation treatment (the temperature is 60 ℃ and the time is 4 hours) to obtain gel, soaking and washing the gel in deionized water to remove unreacted substances, wherein the soaking time is 24 hours, and drying the gel in a 50 ℃ oven to obtain the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for treating heavy metal wastewater.
Example 6
A preparation method of a peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment comprises the following steps:
(1) repeatedly cleaning peanut shells with clear water and deionized water, naturally drying, pulverizing with a pulverizer, and sieving (with 80 mesh sieve) to obtain peanut shell powder;
(2) soaking 25g of the peanut shell powder obtained in the step (1) in 1.0L of hydrochloric acid solution (with the concentration of 1mol/L), stirring for 12 hours, filtering to obtain a precipitate, washing the precipitate to be neutral, and drying in an oven at 50 ℃ to obtain pretreated peanut shell powder;
(3) dissolving 7.0g of sodium hydroxide and 12.0g of urea in 81.0g of water, and uniformly mixing to obtain a mixed solution; adding 9.0g of the pretreated peanut shell powder obtained in the step (2) into the mixed solution, stirring for 12 hours, centrifuging to obtain a supernatant (the centrifugation speed is 8000r/min, and the time is 10min), and obtaining a lignin fiber solution;
(4) adding 5mL of acrylic acid and 5mL of beta-cyclodextrin solution (the concentration is 4 wt%) into 10mL of the lignin fiber solution obtained in the step (3), uniformly mixing, adding 416.0mg of ammonium persulfate and 168.8mg of N, N-methylene-bisacrylamide, and uniformly mixing to obtain a mixed solution;
(5) and (3) transferring the mixed solution obtained in the step (4) into a glass sealed container, heating in a water bath heating mode to carry out gelation treatment (the temperature is 70 ℃ and the time is 3 hours) to obtain gel, soaking and washing the gel in deionized water to remove unreacted substances, wherein the soaking time is 24 hours, and drying the gel in a 50 ℃ oven to obtain the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for treating heavy metal wastewater.
Example 7
A preparation method of a peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment comprises the following steps:
(1) repeatedly cleaning peanut shells with clear water and deionized water, naturally drying, pulverizing with a pulverizer, and sieving (with 80 mesh sieve) to obtain peanut shell powder;
(2) soaking 25g of the peanut shell powder obtained in the step (1) in 1.0L of hydrochloric acid solution (with the concentration of 1mol/L), stirring for 12 hours, filtering to obtain a precipitate, washing the precipitate to be neutral, and drying in an oven at 50 ℃ to obtain pretreated peanut shell powder;
(3) dissolving 7.0g of sodium hydroxide and 12.0g of urea in 81.0g of water, and uniformly mixing to obtain a mixed solution; adding 9.0g of the pretreated peanut shell powder obtained in the step (2) into the mixed solution, stirring for 12 hours, centrifuging to obtain a supernatant (the centrifugation speed is 8000r/min, and the time is 10min), and obtaining a lignin fiber solution;
(4) adding 5mL of acrylic acid and 5mL of beta-cyclodextrin solution (the concentration is 5 wt%) into 10mL of the lignin fiber solution obtained in the step (3), uniformly mixing, adding 416.0mg of ammonium persulfate and 168.8mg of N, N-methylene-bisacrylamide, and uniformly mixing to obtain a mixed solution;
(5) and (3) transferring the mixed solution obtained in the step (4) into a glass sealed container, heating in a water bath heating mode to carry out gelation treatment (the temperature is 70 ℃ and the time is 3 hours) to obtain gel, soaking and washing the gel in deionized water to remove unreacted substances, wherein the soaking time is 24 hours, and drying the gel in a 50 ℃ oven to obtain the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for treating heavy metal wastewater.
Example 8
A preparation method of a peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment comprises the following steps:
(1) repeatedly cleaning peanut shells with clear water and deionized water, naturally drying, pulverizing with a pulverizer, and sieving (with 100 mesh sieve) to obtain peanut shell powder;
(2) soaking 25g of the peanut shell powder obtained in the step (1) in 1.0L of hydrochloric acid solution (the concentration is 1mol/L), stirring for 8 hours, filtering to obtain a precipitate, washing the precipitate to be neutral, and drying in an oven at 50 ℃ to obtain pretreated peanut shell powder;
(3) dissolving 7.0g of sodium hydroxide and 12.0g of urea in 81.0g of water, and uniformly mixing to obtain a mixed solution; adding 9.0g of the pretreated peanut shell powder obtained in the step (2) into the mixed solution, stirring for 8 hours, centrifuging to obtain a supernatant (the centrifugation speed is 8000r/min, and the time is 10min), and obtaining a lignin fiber solution;
(4) adding 5mL of acrylic acid and 5mL of beta-cyclodextrin solution (the concentration is 5 wt%) into 10mL of the lignin fiber solution obtained in the step (3), uniformly mixing, adding 416.0mg of ammonium persulfate and 168.8mg of N, N-methylene-bisacrylamide, and uniformly mixing to obtain a mixed solution;
(5) and (3) transferring the mixed solution obtained in the step (4) into a glass sealed container, heating in a water bath heating mode to carry out gelation treatment (the temperature is 60 ℃ and the time is 4 hours) to obtain gel, soaking and washing the gel in deionized water to remove unreacted substances, wherein the soaking time is 24 hours, and drying the gel in a 50 ℃ oven to obtain the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for treating heavy metal wastewater.
Comparative example 1
This comparative example provides a composite hydrogel material, which was prepared in accordance with example 1, except that no beta-cyclodextrin was added. Fig. 12a and 12b are force diagrams of compression and tensile resistance, respectively, of hydrogel materials synthesized without the addition of beta-cyclodextrin. From the results in FIG. 12a, it can be seen that the gel withstands pressures around 90 kPa; from the results of FIG. 12b, it can be seen that the gel withstands a tensile force of about 16 kPa.
Application example 1
Scanning electron microscopy (scanning electron microscopy result) is carried out on the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment prepared in the example 1;
and (3) drying the synthesized composite hydrogel with a freeze dryer on the cross section to prepare a gel sample, and scanning on an electron microscope after carrying out gold spraying treatment on the surface of the sample. As shown in the Scanning Electron Microscope (SEM) image of fig. 1, the composite hydrogel had a highly interconnected macroporous network and a high crosslink density. The porous structure is beneficial to the diffusion of heavy metal ions to the active sites of the composite gel, and promotes the adsorption of the heavy metal ions.
Application example 2
The peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment prepared in example 2 is subjected to a scanning electron microscope (scanning electron microscope result);
as shown in the Scanning Electron Microscope (SEM) image of fig. 2, the composite hydrogel had a highly interconnected macroporous network and a high crosslinking density as the composite hydrogel synthesized in example 1.
Application example 3
100mg of the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbents prepared in examples 1, 2, 4, 6 and 7 for heavy metal wastewater treatment were weighed and added to 100mL (100 mg. L) of each adsorbent-1) The initial pH value of Cd (II) solution is adjusted to 5.0 +/-0.01,the shaker was placed at 298K and a rotation speed of 180 pm. Shaking in a shaking table for 4h to allow the adsorption reaction to reach equilibrium. And (3) filtering the reacted solution by using a filter membrane, and then testing the content of the residual heavy metal in the solution by adopting flame atomic absorption.
As shown in fig. 3, the composite hydrogel adsorbents synthesized by adding different contents of beta-cyclodextrin have different effects on removing heavy metals, and the beta-cyclodextrin with the content of 1% is more economical and effective to be added as a monomer.
Application example 4
The peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment prepared in example 1 is dried and then subjected to infrared spectrum test (infrared spectrogram result);
as shown in FIG. 4, 3454cm-1The strong absorption peak at the position belongs to-OH or-NH2The stretching vibration of (2) indicates that the surface of the adsorbent can have functional groups such as phenol, alcohol, amino and the like; 2930cm-1The weak absorption peak at (A) is due to the formation of C-H bond, indicating the possibility of-CH3Presence of (a); 1631cm-1The strong absorption peak is attributed to the stretching vibration of C ═ O or C ═ C double bonds, which indicates that the surface of the adsorbent may have aldehyde group, carbonyl group and other functional groups; 1030cm-1The strong absorption peak at (a) is attributed to the tensile vibration of the C — O bond. In conclusion, a great number of functional groups such as oxygen-containing groups (-OH, -COOH, C-O and the like) and amino groups exist on the surface of the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for treating heavy metal wastewater, and the functional groups have great promotion effect on adsorption of heavy metals.
Application example 5
The peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment prepared in example 1 is subjected to an X-ray fluorescence diffraction test (X-ray fluorescence diffraction result);
as shown in the result of fig. 5, the peanut shell lignin/β -cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment has an obvious characteristic diffraction peak when the 2 θ is about 20 °, and the original diffraction peaks of the peanut shell and cyclodextrin disappear, indicating that the synthesized gel composite material has high stability.
Application example 6
The composite hydrogel prepared in example 1 (the peanut shell lignin/beta-cyclodextrin composite hydrogel for heavy metal wastewater treatment) is placed in a universal material testing machine to test the material (mechanical property tests including a compression experiment and a tensile experiment).
Compression experiment at room temperature, a synthesized cylindrical wet composite hydrogel sample (peanut shell lignin/beta-cyclodextrin composite hydrogel for heavy metal wastewater treatment without drying treatment) is placed on a lower plate of a Z020 type universal material testing machine, an upper plate connected with a force transducer is compressed at a compression speed of 1.5mm/min, the test is carried out until the gel is irreversibly crushed, and the maximum pressure which can be borne by the gel at the moment is analyzed. Stretching experiments are mainly carried out at room temperature, newly synthesized dumbbell-shaped (thin sheet) wet composite hydrogel is placed at a clamp of a Z020 type universal material testing machine, and is stretched at a stretching speed of 5mm/min through a force transducer until the material is broken. From the results of FIG. 6a, it can be seen that the gel can withstand pressures of around 150 kPa; from the results of FIG. 6b, it can be seen that the gel can withstand a tensile force of about 35 kPa. The results show that the material has excellent mechanical properties and can be applied to the actual water body environment.
Application example 7
The composite hydrogel prepared in example 5 (the peanut shell lignin/beta-cyclodextrin composite hydrogel for heavy metal wastewater treatment) is placed in a universal material testing machine to carry out a compression experiment test (mechanical property test) on the material.
Compression experiment at room temperature, a synthesized cylindrical wet composite hydrogel sample (peanut shell lignin/beta-cyclodextrin composite hydrogel for heavy metal wastewater treatment without drying treatment) is placed on a lower plate of a Z020 type universal material testing machine, an upper plate connected with a force transducer is compressed at a compression speed of 1.5mm/min, the test is carried out until the gel is irreversibly crushed, and the maximum pressure which can be borne by the gel at the moment is analyzed. As is clear from the results in FIG. 7, the gel withstood a pressure of about 95 kPa.
Application example 8
The composite hydrogel prepared in example 8 (the peanut shell lignin/beta-cyclodextrin composite hydrogel for heavy metal wastewater treatment) is placed in a universal material testing machine to perform tensile test (mechanical property test) on the material.
In the tensile experiment, at room temperature, synthesized dumbbell-shaped (thin sheet) wet composite hydrogel (peanut shell lignin/beta-cyclodextrin composite hydrogel for heavy metal wastewater treatment without drying treatment) is placed at a clamp of a Z020 type universal material testing machine, and is connected by a force cell and stretched at a stretching speed of 5mm/min until the material is broken. From the results of FIG. 8, it is clear that the gel can withstand a tensile force of about 27 kPa.
Application example 9
The composite hydrogel adsorbent prepared in example 1 was subjected to an adsorption performance test;
1000 mg/mL of the solution was prepared in advance-1The stock solutions of Pb and Cd and the experimental solutions were diluted with the stock solutions, and the initial pH of the solutions was adjusted by dropwise addition of 0.1mol of HCl or NaOH solution. The set condition parameters are as follows: temperature 298K, shaker rotation speed: 180 pm; the initial pH of the solution was set to 5. + -. 0.01.
(1) Adsorption effect of composite hydrogel material on Pb (II) by adding amount
10mg, 17.5mg, 25mg, 35mg and 50mg of peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment are respectively weighed and added with 50mL (200 mg. L)-1) The solution of Pb (II) was shaken in a shaker for 4 hours to allow the adsorption reaction to reach equilibrium. And (3) filtering the reacted solution by using a filter membrane, and then testing the content of the residual heavy metal in the solution by adopting flame atomic absorption.
As shown in FIG. 9, when Pb (II) is 50mL, the adsorbent content is 17.5mg or more, and 200 mg. L-1Has a removal rate of 99% or more; and when the content of the adsorbent is more than 17.5mg, the adsorption capacity for Pb (II) can approach 400 mg/g. The optimum amount of the adsorbent to be used is 0.5g/L in combination.
(2) Study on adsorption kinetics of composite hydrogel material on Pb (II), Cd (II)
Are respectively provided with50mg of hydrogel was weighed and added to 100mL (100 mg. L) of each-1) In Pb (II), Cd (II) solution for 1min, 2min, 4min, 6min, 8min, 10min, 20min, 40min, 60min, 80min, 120min, 160min, 200 min. 0.5ml of the solution was taken each time and filtered through a filter head, and the heavy metal concentration of the taken solution was measured by a flame atomic absorption method.
As shown by the results of FIG. 10a and FIG. 10b, the material has high adsorption efficiency on Pb (II) and Cd (II), and can reach adsorption equilibrium within 120min, wherein the adsorption capacity is 160mg/g and 100mg/g respectively.
(3) Composite hydrogel adsorbent for Cd with different concentrations2+Adsorption rate and adsorption capacity of
Respectively weighing 20mg of composite hydrogel material, adding 40mL of composite hydrogel material with different concentrations (10 mg. L)-1、25mg·L-1、50mg·L-1、100mg·L-1And 150 mg. L-1) Cd (2)2+The solution was shaken in a shaker for 4h to allow the adsorption reaction to equilibrate. And filtering the obtained solution by a filter head, and measuring the concentration of heavy metal in the solution by adopting a flame atomic absorption method.
As the results in FIG. 11 show, the adsorbent was used even at the initial Cd2+When the concentration is as high as 150mg/L, the maximum adsorption capacity can reach 146mg/g respectively.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of a peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment is characterized by comprising the following steps:
(1) crushing peanut shells, and sieving to obtain peanut shell powder;
(2) soaking the peanut shell powder in the step (1) in a hydrochloric acid solution, stirring, filtering to obtain a precipitate, washing the precipitate to be neutral, and drying to obtain pretreated peanut shell powder;
(3) dissolving sodium hydroxide and urea in water, and uniformly mixing to obtain a mixed solution; adding the pretreated peanut shell powder obtained in the step (2) into the mixed solution, stirring, centrifuging and taking supernatant to obtain a lignin fiber solution;
(4) adding acrylic acid and a beta-cyclodextrin solution into the lignin fiber solution obtained in the step (3), uniformly mixing, adding ammonium persulfate and N, N-methylene bisacrylamide, and uniformly mixing to obtain a mixed solution;
(5) and (4) heating the mixed solution obtained in the step (4) to carry out water bath heating treatment to obtain gel, washing and drying to obtain the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for treating heavy metal wastewater.
2. The preparation method of the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment as claimed in claim 1, wherein the size of the sieve in step (1) is 60-100 meshes.
3. The preparation method of the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment according to claim 1, wherein the concentration of the hydrochloric acid solution in the step (2) is 0.5-1.0 mol/L; the mass volume ratio of the peanut shell powder to the hydrochloric acid solution is 20-30: 1 g/L; the stirring treatment time is 8-16 h.
4. The preparation method of the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment according to claim 1, wherein the mass ratio of the sodium hydroxide, the urea and the water in the step (3) is (5-10): (10-15): (75-85).
5. The preparation method of the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment according to claim 1, wherein the mass ratio of the pretreated peanut shell powder to the mixed solution in the step (3) is (8-15): (80-120); the stirring treatment time is 8-16 h.
6. The preparation method of the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment as claimed in claim 1, wherein the rotation speed of the centrifugation in the step (3) is 8000-10000r/min, and the centrifugation time is 5-15 min.
7. The preparation method of the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment according to claim 1, wherein the cyclodextrin solution in the step (4) is 1-5% by mass; the volume ratio of the lignin fiber solution to the acrylic acid and cyclodextrin solution is (6-16): (3-8): (3-8); the molar ratio of the acrylic acid, the ammonium persulfate and the N, N-methylene-bisacrylamide in the step (4) is 100: (0.1-0.25): (1-2).
8. The preparation method of the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment according to claim 1, wherein the temperature of the water bath heating treatment in the step (5) is 50-70 ℃, and the time of the water bath heating treatment is 2-4 h; the washing comprises the following steps: soaking the gel in deionized water for 12-24h, taking out, and washing the gel with water again; the drying temperature is 50-60 ℃.
9. A peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment prepared by the preparation method of any one of claims 1-8.
10. The use of the peanut shell lignin/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment as claimed in claim 9 as a heavy metal adsorbent for treating polluted wastewater.
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