CN113368831B - Kaolin-nano Fe 2 O 3 -lignin hydrogel composite material and preparation method and application thereof - Google Patents
Kaolin-nano Fe 2 O 3 -lignin hydrogel composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses kaolin-nano Fe 2 O 3 A lignin hydrogel composite material, a preparation method and application thereof, belonging to the technical field of composite materials. The kaolin-nano Fe 2 O 3 -a method of preparing a lignin hydrogel composite comprising: (1) Taking kaolin and nano ferric oxide, adding water, stirring and dissolving to obtain a mixed solution 1; (2) Adding acrylamide, maleic anhydride, sodium lignosulfonate and N, N' -methylene bisacrylamide into the mixed solution 1 obtained in the step (1) to obtain a mixed solution 2; (3) Adjusting the pH value of the mixed solution 2 obtained in the step (2), adding an initiator and a cross-linking agent, stirring, standing, freezing, and freeze-drying to obtain the kaolin-nano Fe 2 O 3 -a lignin hydrogel composite. The method disclosed by the invention is simple and convenient to operate, stable in structure and strong in adsorption performance, and can be used for better removing heavy metals, especially heavy metal cadmium, from a polluted environment.
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to kaolin-nano Fe 2 O 3 -lignin hydrogel composite material and preparation method and application thereof.
Background
Heavy metal is one of pollution sources which have the widest pollution range and the greatest harm in natural ecological environment, and people pay more and more attention to the heavy metal. Heavy metal pollution seriously affects the growth and development of plants, the yield and the quality of crops, and is transmitted into human bodies through biological chains, thus seriously harming human health. Cadmium (Cd) is a heavy metal element with strong toxicity to human health, and can seriously threaten human health through a food chain due to high biological activity and strong toxicity. In recent years, the problems of Cd pollution of farmland soil in China and Cd pollution of rice caused by the Cd pollution are highly concerned by the public. Therefore, experts and scholars call for timely treatment of cadmium pollution in farmland to avoid causing greater harm.
In recent years, relevant experts propose effective treatment methods such as passivator remediation, super-accumulation plant absorption, low-accumulation crop screening and the like for farmland heavy metal pollution. However, these methods cannot remove heavy metals fundamentally, and have the problems of poor persistence, secondary pollution, destruction of soil structures and biological communities, and the like. The adsorption method, which uses a substance with a large specific surface area as an adsorbent and has surface atoms with high activity, is a priority for effectively removing cadmium from the environment, and the surface atoms combine the adsorbent with heavy metals through physicochemical adsorption, oxidation reduction and other means, thereby reducing the bioavailability of the heavy metals. The adsorption method is a simple, convenient and mature method. In this regard, how to effectively utilize the adsorbent having high adsorption performance is the key of the present stage.
The nano ferric oxide has good heavy metal adsorption performance, but is easy to agglomerate and difficult to recover after being used. The high-performance application and recovery of the hydrogel can be realized by loading the hydrogel with the hydrogel. The hydrogel is a hydrophilic material with high water absorption and high water retention performance. It can provide carrier, enrich heavy metal, can separate and recover, especially suitable for the soil cadmium reduction of the paddy field. However, the nano ferric oxide has high reactivity, so that a monomer in hydrogel synthesis is inactivated, and the loading of the hydrogel cannot be realized. Therefore, how to combine the nano ferric oxide with the hydrogel to be applied to heavy metal adsorption is very important.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide kaolin-nano Fe 2 O 3 A method for preparing a lignin hydrogel composite.
The second purpose of the invention is to provide the kaolin-nano Fe prepared by the method 2 O 3 -a lignin hydrogel composite.
The third purpose of the invention is to provide the kaolin-nano Fe 2 O 3 -use of a lignin hydrogel composite.
The purpose of the invention is realized by the following technical scheme:
kaolin-nano Fe 2 O 3 -a method for preparing a lignin hydrogel composite comprising the steps of:
(1) Adding kaolin and nano ferric oxide into water, stirring and dissolving to obtain a mixed solution 1;
(2) Adding acrylamide, maleic anhydride, sodium lignosulphonate and N, N' -methylene bisacrylamide into the mixed solution 1 obtained in the step (1) to obtain a mixed solution 2;
(3) Adjusting the pH value of the mixed solution 2 obtained in the step (2) to 5-8Adding initiator and cross-linking agent, stirring, standing, freezing, freeze-drying to obtain kaolin-nano Fe 2 O 3 -a lignin hydrogel composite.
In the step (1), the kaolin and the nano ferric oxide are preferably calculated according to the mass ratio of 1.00-10.00; more preferably, the mass ratio is 2.00 to 8.00.
In the step (1), the kaolin and the water are preferably calculated according to the mass (g) volume (mL) ratio of 1.00-10.00; more preferably, the mass (g) to volume (mL) ratio is from 2.00 to 8.00.
In the step (1), the water is preferably at least one of distilled water, deionized water and ultrapure water; more preferably deionized water.
In the step (1), the stirring is preferably magnetic stirring.
In the step (2), the acrylamide, the maleic anhydride, the sodium lignosulfonate, the N, N' -methylene bisacrylamide and the kaolin are preferably calculated according to the mass ratio of 1.00-8.00; more preferably, the mass ratio is 2.00 to 8.00.
In the step (3), the reagent for adjusting pH is preferably sodium hydroxide.
In the step (3), the mass ratio of the maleic anhydride to the initiator is preferably 0.50-4.00; more preferably, the mass ratio is 0.50 to 3.55.
In the step (3), the initiator is preferably potassium persulfate.
In the step (3), the ratio of the maleic anhydride to the cross-linking agent is preferably calculated according to mass (g) to volume (mu L) of 0.50-4.00; more preferably, it is calculated in a mass (g) to volume (μ L) ratio of 0.50 to 3.55.
In the step (3), the cross-linking agent is preferably tetramethylethylenediamine.
In the step (3), the standing time is preferably 2 to 12 hours.
In the step (3), the freezing condition is preferably-20 to-10 ℃ for 2 to 12 hours; more preferably-20 to-10 ℃ for 12 hours.
In the step (3), the freeze-drying time is preferably 12 to 24 hours.
Kaolin-nano Fe 2 O 3 -a lignin hydrogel composite material, prepared by the above preparation method.
The kaolin-nano Fe 2 O 3 Application of the lignin hydrogel composite in the field of removal of heavy metals, in particular in water and/or soil.
The heavy metal is cadmium.
The preparation method of the invention has the following advantages and beneficial effects:
(1) The raw materials of the invention are sodium lignosulfonate and kaolin, which are rich in sources, economical and practical, reduce resource waste and are environment-friendly.
(2) The preparation method is simple, can be completed by simple mixing, has no secondary pollution to the environment, and is safe and environment-friendly.
(3) The kaolin-nano Fe of the invention 2 O 3 The nano Fe can be effectively added by adding the kaolin in the preparation process of the lignin hydrogel composite material 2 O 3 Dispersing to avoid agglomeration in gel, and greatly improving the nano Fe 2 O 3 The utilization ratio of (2). And the influence on the synthesis of free radicals by the gel is avoided, so that the hydrogel is smoothly synthesized in one step.
(4) The invention uses kaolin as a dispersing agent of nano ferric oxide, and the kaolin is coated and then combined with hydrogel to construct a novel kaolin-nano Fe 2 O 3 The lignin hydrogel composite material simply realizes the dispersion and loading of the nano ferric oxide, is convenient to use and recover, and reduces the environmental load.
(5) The method disclosed by the invention is simple and convenient to operate, stable in structure and strong in adsorption performance, and can be used for well removing heavy metals, especially heavy metal cadmium, from a polluted environment.
Drawings
FIG. 1 shows the Kaolin-nano Fe prepared in example 7 2 O 3 -a comparison of the lignin hydrogel composite before and after water absorption;
FIG. 2 is a diagram showing the adsorption effect of heavy metal Cd by different materials; wherein: number 1 refers to sodium lignosulfonate; number 2 refers to kaolin; no. 3 indicates nano Fe 2 O 3 (ii) a No. 4 refers to the lignin hydrogel of comparative example 1; no. 5 refers to the kaolin-lignin hydrogel composite of comparative example 2; no. 6 indicates that the nano Fe of comparative example 3 2 O 3 -a lignin hydrogel composite; number 7 refers to the kaolin-nano Fe of example 7 2 O 3 -a lignin hydrogel composite.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Kaolin clay was purchased from Shanghai Aladdin Biotechnology Ltd.
Example 1
Kaolin-nano Fe 2 O 3 -a method for preparing a lignin hydrogel composite comprising the steps of:
(1) Taking 2.00g of kaolin and 0.50g of nano ferric oxide, adding 20mL of deionized water, magnetically stirring, and completely dissolving to obtain a mixed solution 1;
(2) Adding 2.00g of acrylamide, 0.50g of maleic anhydride, 0.35g of sodium lignosulfonate and 0.02g of N, N' -methylene bisacrylamide into the mixed solution 1 obtained in the step (1) to obtain a mixed solution 2;
(3) Adding 0.50g of sodium hydroxide into the mixed solution 2 obtained in the step (2), adjusting the pH value to 5-8, adding 0.05g of potassium persulfate serving as an initiator, adding 60 mu L of cross-linking agent tetramethylethylenediamine, fully stirring, standing for 2h, putting into a refrigerator, freezing at-10 ℃ for 12h, and freeze-drying for 24h to obtain the kaolin-nano Fe 2 O 3 -a lignin hydrogel composite.
Example 2
Kaolin-nano Fe 2 O 3 -a method for preparing a lignin hydrogel composite comprising the steps of:
(1) Adding 3.50g of kaolin and 1.00g of nano ferric oxide into 40mL of deionized water, and magnetically stirring and completely dissolving to obtain a mixed solution 1;
(2) Adding 3.50g of acrylamide, 2.50g of maleic anhydride, 0.44g of sodium lignosulfonate and 0.04g of N, N' -methylene bisacrylamide into the mixed solution 1 obtained in the step (1) to obtain a mixed solution 2;
(3) Adding 1.00g of sodium hydroxide into the mixed solution 2 obtained in the step (2), adjusting the pH value to 5-8, adding 0.10g of potassium persulfate serving as an initiator, adding 70 mu L of cross-linking agent tetramethylethylenediamine, fully stirring, standing for 4h, putting into a refrigerator, freezing at-20 ℃ for 12h, and freeze-drying for 24h to obtain the kaolin-nano Fe 2 O 3 -a lignin hydrogel composite.
Example 3
Kaolin-nano Fe 2 O 3 -a method for preparing a lignin hydrogel composite comprising the steps of:
(1) Adding 5.00g of kaolin and 1.35g of nano ferric oxide into 60mL of deionized water, and magnetically stirring and completely dissolving to obtain a mixed solution 1;
(2) Adding 4.00g of acrylamide, 2.00g of maleic anhydride, 2.44g of sodium lignosulfonate and 0.15g of N, N' -methylene bisacrylamide into the mixed solution 1 obtained in the step (1) to obtain a mixed solution 2;
(3) Adding 1.50g of sodium hydroxide into the mixed solution 2 obtained in the step (2), adjusting the pH value to 5-8, adding 0.15g of potassium persulfate serving as an initiator, adding 80 mu L of cross-linking agent tetramethylethylenediamine, fully stirring, standing for 5h, putting into a refrigerator, freezing at-15 ℃ for 12h, and freeze-drying for 12h to obtain the kaolin-nano Fe 2 O 3 -a lignin hydrogel composite.
Example 4
Kaolin-nano Fe 2 O 3 -a method for preparing a lignin hydrogel composite comprising the steps of:
(1) Taking 5.58g of kaolin and 2.84g of nano ferric oxide, adding 70mL of deionized water, and magnetically stirring to dissolve completely to obtain a mixed solution 1;
(2) Adding 5.05g of acrylamide, 1.85g of maleic anhydride, 2.85g of sodium lignosulfonate and 0.20g of N, N' -methylene bisacrylamide into the mixed solution 1 obtained in the step (1) to obtain a mixed solution 2;
(3) Adding 2.00g of sodium hydroxide into the mixed solution 2 obtained in the step (2), adjusting the pH value to 5-8, adding 0.15g of potassium persulfate serving as an initiator, adding 100 mu L of cross-linking agent tetramethylethylenediamine, fully stirring, standing for 5h, putting into a refrigerator, freezing at-20 ℃ for 12h, and freeze-drying for 24h to obtain the kaolin-nano Fe 2 O 3 -a lignin hydrogel composite.
Example 5
Kaolin-nano Fe 2 O 3 -a method for preparing a lignin hydrogel composite comprising the steps of:
(1) Taking 8.00g of kaolin and 3.15g of nano ferric oxide, adding 60mL of deionized water, and magnetically stirring to dissolve completely to obtain a mixed solution 1;
(2) Adding 5.05g of acrylamide, 2.00g of maleic anhydride, 3.00g of sodium lignosulfonate and 0.40g of N, N' -methylene bisacrylamide into the mixed solution 1 obtained in the step (1) to obtain a mixed solution 2;
(3) Adding 2.00g of sodium hydroxide into the mixed solution 2 obtained in the step (2), adjusting the pH value to 5-8, adding 0.20g of potassium persulfate serving as an initiator, adding 110 mu L of cross-linking agent tetramethylethylenediamine, fully stirring, standing for 6h, freezing for 12h at-20 ℃ in a refrigerator, and freeze-drying for 24h to obtain the kaolin-nano Fe 2 O 3 -a lignin hydrogel composite.
Example 6
Kaolin-nano Fe 2 O 3 -a method for preparing a lignin hydrogel composite comprising the steps of:
(1) Taking 6.65g of kaolin and 2.45g of nano ferric oxide, adding 80mL of deionized water, and magnetically stirring to dissolve completely to obtain a mixed solution 1;
(2) Adding 8.00g of acrylamide, 3.55g of maleic anhydride, 3.85g of sodium lignosulfonate and 0.50g of N, N' -methylene bisacrylamide into the mixed solution 1 obtained in the step (1) to obtain a mixed solution 2;
(3) Adding 1.50g of sodium hydroxide into the mixed solution 2 obtained in the step (2), adjusting the pH value to 5-8, adding 0.50g of potassium persulfate serving as an initiator and 120 mu L of tetramethylethylenediamine serving as a cross-linking agent, fully stirring, standing for 6h, putting into a refrigerator, freezing at-20 ℃ for 12h, and freeze-drying for 12h to obtain the kaolin-nano Fe 2 O 3 -a lignin hydrogel composite.
Example 7
Kaolin-nano Fe 2 O 3 -a method for preparing a lignin hydrogel composite comprising the steps of:
(1) Taking 8.00g of kaolin and 2.00g of nano ferric oxide, adding 60mL of deionized water, magnetically stirring and completely dissolving to obtain a mixed solution 1;
(2) Adding 8.00g of acrylamide, 3.35g of maleic anhydride, 0.85g of sodium lignosulfonate and 0.25g of N, N' -methylene bisacrylamide into the mixed solution 1 obtained in the step (1) to obtain a mixed solution 2;
(3) Adding 2.00g of sodium hydroxide into the mixed solution 2 obtained in the step (2), adjusting the pH value to 5-8, adding 0.20g of potassium persulfate serving as an initiator, adding 110 mu L of cross-linking agent tetramethylethylenediamine, fully stirring, standing for 12h, freezing for 12h at-20 ℃ in a refrigerator, and freeze-drying for 24h to obtain the kaolin-nano Fe 2 O 3 -a lignin hydrogel composite.
Comparative example 1
A preparation method of lignin hydrogel comprises the following steps:
(1) Taking 8.00g of acrylamide, 3.35g of maleic anhydride, 0.85g of sodium lignosulfonate and 0.25g of N, N' -methylene bisacrylamide, adding 60mL of deionized water, and completely dissolving by magnetic stirring to obtain a mixed solution;
(2) And (2) adding 2.00g of sodium hydroxide into the mixed solution obtained in the step (1), adjusting the pH value to 5-8, adding 0.20g of potassium persulfate serving as an initiator, adding 110 mu L of cross-linking agent tetramethylethylenediamine, fully stirring, standing for 12h, freezing in a refrigerator at-20 ℃ for 12h, and freeze-drying for 24h to obtain the lignin hydrogel.
Comparative example 2
A preparation method of kaolin-lignin hydrogel composite material comprises the following steps:
(1) Taking 8.00g of kaolin, 8.00g of acrylamide, 3.35g of maleic anhydride, 0.85g of sodium lignosulfonate and 0.25g of N, N' -methylene bisacrylamide, adding 60mL of deionized water, and magnetically stirring to completely dissolve the materials to obtain a mixed solution;
(2) Adding 2.00g of sodium hydroxide into the mixed solution obtained in the step (1), adjusting the pH value to 5-8, adding 0.20g of potassium persulfate serving as an initiator, adding 110 mu L of cross-linking agent tetramethylethylenediamine, fully stirring, standing for 12h, putting into a refrigerator, freezing at-20 ℃ for 12h, and freeze-drying for 24h to obtain the kaolin-lignin hydrogel composite material.
Comparative example 3
Nano Fe 2 O 3 -a method for preparing a lignin hydrogel composite comprising the steps of:
(1) Taking 2.00g of nano ferric oxide, 8.00g of acrylamide, 3.35g of maleic anhydride, 0.85g of sodium lignosulfonate and 0.25g of N, N' -methylene bisacrylamide, adding 60mL of deionized water, and magnetically stirring to completely dissolve to obtain a mixed solution;
(2) Adding 2.00g of sodium hydroxide into the mixed solution obtained in the step (1), adjusting the pH value to 5-8, adding 0.20g of potassium persulfate serving as an initiator, adding 110 mu L of cross-linking agent tetramethylethylenediamine, fully stirring, standing for 12h, putting into a refrigerator, freezing at-20 ℃ for 12h, and freeze-drying for 24h to obtain the nano Fe 2 O 3 -a lignin hydrogel composite.
Measurement of Performance
(1) Water absorption test
The kaolin obtained in example 7 is mixed with nano Fe 2 O 3 After the lignin hydrogel composite material is put into water to absorb water for 48 hours, kaolin-nano Fe before and after water absorption is calculated 2 O 3 -weight of lignin hydrogel composite, calculating the water absorption of the composite, i.e. water absorption (%) = (mass after water absorption-mass before water absorption)/mass before water absorptionMass X100%.
Kaolin-nano Fe before and after water absorption 2 O 3 The lignin hydrogel composite is shown in figure 1. Tests prove that the kaolin-nano Fe obtained in example 7 2 O 3 The water absorption of the lignin hydrogel composite was 430%.
(2) Adsorption experiments
0.85g of sodium lignosulfonate, 8.00g of kaolin, 2.00g of nano ferric oxide, the lignin hydrogel of comparative example 1, the kaolin-lignin hydrogel composite material of comparative example 2 and the nano Fe of comparative example 3 are respectively added 2 O 3 Lignin hydrogel composite, kaolin-NanFei from example 7 2 O 3 Adding 0.0300g (+ -0.0050 g) of each lignin hydrogel composite material into 30mL of 50ppm Cd (II) solution, repeating twice, putting the solution into a shaking table for 180 revolutions, adsorbing for 5 hours, filtering by using a 0.45-micrometer inorganic filter head, and diluting to 1ppm to obtain an adsorption solution. Measuring the concentration of Cd (II) in the adsorption solution by using an atomic absorption spectrophotometer, and calculating the adsorption capacity of Cd (II) according to the following formula:
wherein q is t Expressing the adsorption quantity of the material after adsorbing for a certain time, and the unit is mg/g; c 0 Represents the initial concentration of Cd (II) in mg/L; c t Expressing the concentration of Cd (II) solution after adsorbing for a certain time in mg/L; m represents the mass of the composite material in g; v represents the volume of Cd (II) solution in units of L.
The results are shown in FIG. 2. As can be seen from FIG. 2, the kaolin obtained in example 7-nano Fe 2 O 3 The lignin hydrogel composite material shows better adsorption effect on heavy metal Cd, which shows that the kaolin-nano Fe prepared by the method of the invention 2 O 3 The components in the lignin hydrogel composite material have a synergistic effect on the adsorption of heavy metal Cd.
In addition, it was found through experiments that the kaolin prepared in examples 1-6Nano Fe 2 O 3 The adsorption capacity of the lignin hydrogel composite to cadmium is similar to that of example 7.
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 (8)
1. Kaolin-nano Fe 2 O 3 -a method for preparing a lignin hydrogel composite, characterized in that it comprises the following steps:
(1) Adding kaolin and nano ferric oxide into water, stirring and dissolving to obtain a mixed solution 1;
(2) Adding acrylamide, maleic anhydride, sodium lignosulphonate and N, N' -methylene bisacrylamide into the mixed solution 1 obtained in the step (1) to obtain a mixed solution 2;
(3) Adjusting the pH value of the mixed solution 2 obtained in the step (2) to 5~8, adding an initiator, adding a cross-linking agent, stirring, standing, freezing, and freeze-drying to obtain the kaolin-nano Fe 2 O 3 -a lignin hydrogel composite;
in the step (1), the kaolin and the nano ferric oxide are calculated according to the mass ratio of (1.00-10.00) to (0.50-5.00);
in the step (1), the kaolin and the water are calculated according to the mass-to-volume ratio (1.00-10.00) g (20-100) mL;
in the step (2), the acrylamide, the maleic anhydride, the sodium lignosulfonate, the N, N' -methylene bisacrylamide and the kaolin are calculated according to the mass ratio of (1.00-8.00) to (0.50-4.00) to (0.35-5.00) to (0.02-2.00) to (1.00-10.00);
in the step (3), the initiator is potassium persulfate;
in the step (3), the cross-linking agent is tetramethylethylenediamine;
in the step (3), the maleic anhydride and the initiator are calculated according to the mass ratio of (0.50-4.00) to (0.05-1.00);
in the step (3), the maleic anhydride and the cross-linking agent are calculated according to the mass-to-volume ratio (0.50-4.00) g, (60-120) mu L.
2. The production method according to claim 1,
the kaolin and the nano ferric oxide are calculated according to the mass ratio of (2.00-8.00) to (0.50-3.15);
the kaolin and the water are calculated according to the mass volume ratio (2.00-8.00) g (20-80) mL.
3. The production method according to claim 1,
the mass ratio of the acrylamide, the maleic anhydride, the sodium lignosulfonate, the N, N' -methylene bisacrylamide and the kaolin is (2.00-8.00), (0.50-3.55), (0.35-3.85), (0.02-0.50) and (2.00-8.00);
the mass ratio of the maleic anhydride to the initiator is (0.50-3.55) to (0.05-0.50);
the maleic anhydride and the cross-linking agent are calculated according to the mass-volume ratio (0.50-3.55) g (60-120) mu L.
4. The production method according to claim 1,
in the step (1), the water is at least one of distilled water, deionized water and ultrapure water;
in the step (3), the reagent for adjusting the pH is sodium hydroxide.
5. The production method according to claim 1,
in the step (3), the standing time is 2-12 h;
in the step (3), the freezing condition is that the freezing is carried out for 2 to 12 hours at the temperature of between 20 ℃ below zero and 10 ℃ below zero;
in the step (3), the freeze drying time is 12-24 h.
6. Kaolin-nano Fe 2 O 3 -a lignin hydrogel composite, characterized in that it is prepared by the preparation method according to any one of claims 1 to 5.
7. Kaolin-nano Fe of claim 6 2 O 3 Application of the lignin hydrogel composite in the field of heavy metal removal.
8. The use according to claim 7,
the heavy metal is the heavy metal in the water body and/or the soil;
the heavy metal is cadmium.
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