CN110523399B - Preparation method and application of chitosan/mica/PEI composite material - Google Patents
Preparation method and application of chitosan/mica/PEI composite material Download PDFInfo
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- CN110523399B CN110523399B CN201910859040.4A CN201910859040A CN110523399B CN 110523399 B CN110523399 B CN 110523399B CN 201910859040 A CN201910859040 A CN 201910859040A CN 110523399 B CN110523399 B CN 110523399B
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/106—Selenium compounds
Abstract
The invention provides a preparation method of a chitosan/mica/PEI composite material, which relates to the technical field of composite material preparation, and the preparation process of the preparation method of the chitosan/mica/PEI composite material comprises the following steps: (1) preparing a chitosan acetic acid solution, (2) preparing a chitosan/mica composite material, and (3) preparing a chitosan/mica/PEI composite material; the invention takes a chitosan/acetic acid system regenerated composite material as a research object, prepares a chitosan/mica modified composite material by a physical blending method, then takes epoxy chloropropane as a cross-linking agent to react with polyethyleneimine to prepare a novel chitosan/mica/PEI organic-inorganic composite material, and applies the novel chitosan/mica/PEI organic-inorganic composite material to adsorb Se (IV) in selenious acid, and collects and recycles the excessive Se (IV) in water, thereby not only solving the danger problem of selenium, but also being used as a controlled release selenium fertilizer after proper treatment.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of composite material preparation, in particular to a preparation method and application of a chitosan/mica/PEI composite material.
[ background of the invention ]
Selenium (Selenium, Se) is a trace element essential for life, is an essential component of selenocysteine and Selenium-containing enzymes such as peroxidase, and plays an important role in anticancer, antioxidation and the like. Researches show that the selenium can resist the damage of free radicals in plants, promote the growth and development of the plants, resist heavy metals and improve the stress resistance of the plants. The selenium with different forms as feed additive has effects of promoting growth and development of aquatic organism, and improving immunity and oxidation resistance.
However, selenious acid and its salt have strong biological toxicity, strong water solubility, easy loss and the like. With the wide application of selenium in the electronic industry and agriculture, serious pollution is caused to the ecological environment due to improper use and excessive discharge of selenium. At present, an adsorption method is one of the main methods for removing selenious acid and Se (IV) salt thereof in water bodies due to convenient operation and good separation effect. And the selenium source adsorbed on the degradable material can be used as a nutrient in the selenium-deficient soil or an additive for the selenium source. Therefore, the excessive Se (IV) in the water body is collected and reused by adopting an adsorption method, so that the danger problem of selenium can be solved, and the selenium fertilizer can be used as the selenium fertilizer after proper treatment.
The molecular structure of chitosan contains a large amount of amine groups and carboxyl groups, so that the chitosan also has good adsorption effect on heavy metals, however, the chitosan is easy to degrade and unstable under acidic conditions due to weak mechanical properties, and the application of the chitosan is limited. The modified chitosan is obtained by modifying amido and hydroxyl on a chitosan molecular chain through chemical reaction, and because the lone pair of electrons on the amido nitrogen atom has good nucleophilicity, the research on the amido chemical modification of the chitosan molecule is more.
However, these modifications are disadvantageous in improving the adsorption performance of chitosan as an adsorbent. Firstly, the chitosan is modified through amino group reaction, so that the number of amino groups capable of being quaternized is reduced, the adsorption capacity is reduced, and the adsorption material is not easy to separate from a water body along with the increase of water solubility.
As a natural polymer, the adsorption performance of chitosan is affected by its own physical form, degree of deacetylation and pH value of the system. Therefore, physical and chemical modification of chitosan is a necessary means for improving the adsorption performance of chitosan and expanding the application range. At present, chitosan composite is more applied in the aspect of adsorbing heavy metal ions, the technology is mature, but the research on Se (IV) adsorption performance is rarely reported.
Therefore, research and development of a proper Se (IV) adsorbent have positive significance for preventing potential harm and collecting and recycling the Se (IV) adsorbent.
[ summary of the invention ]
In view of the above, the invention aims to provide a preparation method of a chitosan/mica/PEI composite material, which takes a chitosan/acetic acid system regenerated composite material as a research object, prepares a chitosan/mica modified composite material by a physical blending method, and then takes epoxy chloropropane as a cross-linking agent to react with polyethyleneimine to prepare a novel chitosan/mica/PEI organic-inorganic composite material.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a chitosan/mica/PEI composite material comprises the following steps:
(1) preparing a chitosan acetic acid solution: weighing 0.3-0.35g of chitosan, and dissolving the chitosan in 8-12mL of dilute acetic acid solution to obtain chitosan acetic acid solution for later use;
(2) preparing a chitosan/mica composite material: adding mica powder with the mass ratio of 1:1-4 to chitosan into a chitosan acetic acid solution, stirring and fully dissolving the mica powder, transferring the mixture into an injector, then dropping the solution in the injector into a NaOH solution to form small balls, taking out the small balls after coagulation, filtering and washing the small balls to be neutral, and then drying the small balls to obtain a chitosan/mica composite material for later use;
(3) preparing a chitosan/mica/PEI composite material: adding 7-9mL of distilled water and 0.3-0.7mL of epoxy chloropropane into 1-2mL of polyethyleneimine, fully stirring the three to uniformly mix the mixture to obtain a soaking solution, then putting the chitosan/mica composite material into the soaking solution to soak for 4-6h, then taking the chitosan/mica composite material out of the soaking solution, putting the chitosan/mica composite material into a 50-60 ℃ drying oven to fully react for 11-13h, and then putting the drying oven into a freeze dryer to dry, thus obtaining the chitosan/mica/PEI composite material.
In the present invention, further, the amount of chitosan in the step (1) is preferably 0.32g, and the amount of diluted acetic acid is preferably 10 mL.
In the present invention, further, the mass ratio of the mica powder to the chitosan in the step (2) is preferably 1: 2.
In the invention, further, the concentration of the dilute acetic acid solution in the step (1) is 2%.
In the present invention, the amount of polyethyleneimine, the amount of distilled water and the amount of epichlorohydrin in the soaking solution of step (3) are preferably 1.5mL, 8mL and 0.5mL, respectively.
In the invention, further, the concentration of the NaOH solution in the step (2) is 1 mol/L.
In the present invention, further, the freeze-drying in the step (3) is drying at a temperature of-50 ℃ for 24 hours.
In the invention, further, in the step (3), the chitosan/mica composite material is placed in the soaking solution for soaking for 5 hours, and then the chitosan/mica composite material is taken out of the soaking solution and placed in a 55 ℃ oven to be fully reacted for 12 hours.
The invention also provides an application of the chitosan/mica/PEI composite material, which comprises an application of Se (IV) in selenious acid adsorption, and the best adsorption condition is obtained through a large number of experimental researches: the temperature is 50 ℃, the pH is 3 and the adsorption time is 2 h.
In summary, due to the adoption of the technical scheme, the invention at least comprises the following beneficial effects:
1. the production process of the invention has the advantages of short flow, simple operation condition, simple steps for completing the preparation process, low production cost, simple required equipment and easy realization of large-scale production.
2. The invention takes a chitosan/acetic acid system regenerated composite material as a research object, prepares a chitosan/mica modified composite material by a simple physical blending method, then takes epoxy chloropropane as a cross-linking agent to react with Polyethyleneimine (PEI) to prepare a novel chitosan/mica/PEI organic-inorganic composite material, and applies the novel chitosan/mica/PEI organic-inorganic composite material to adsorb Se (IV) in selenious acid, collects and reuses the excessive Se (IV) in water, not only can solve the dangerous problem of selenium, but also can be used as a selenium fertilizer after proper treatment; obtaining the composition proportion with the best adsorption effect through a plurality of tests; the effect of each factor on Se (IV) adsorption capacity was then investigated by using a single factor experiment. The adsorption capacity of the C2M1/PEI composite material is the best, and when the initial concentration is 100mg/L, pH-3, the adsorption time is 2h, and the temperature is 50 ℃, the adsorption equilibrium capacity of the C2M1/PEI composite material is the best, and the removal rate of Se (IV) is the highest. The method lays a certain foundation for the research and practical application of adsorbing Se (IV) in the solution based on the chitosan-mica composite material, and has outstanding substantive characteristics and remarkable progress.
[ description of the drawings ]
FIG. 1 is a Se (IV) standard curve diagram
FIG. 2 is a graph of the effect of composite materials of different chitosan ratios on Se (IV) adsorption;
FIG. 3 is a graph showing the effect of different pH values on Se (IV) adsorption of a composite material;
FIG. 4 is a graph showing the effect of mica and optimized ratios of ternary composites C2M1/PEI on Se (IV) adsorption;
FIG. 5 is a graph of the effect of C2M1/PEI on Se (IV) adsorption at different temperatures.
The attached figure analysis is shown in the test and the result analysis.
[ detailed description ] embodiments
The following examples may help one skilled in the art to more fully understand the present invention, but are not intended to limit the invention in any way.
Example 1
The embodiment provides a preparation method of a chitosan/mica/PEI composite material, which comprises the following steps:
(1) preparing a chitosan acetic acid solution: weighing 0.3g of chitosan, and dissolving the chitosan in 8mL of dilute acetic acid solution with the concentration of 2% to obtain chitosan acetic acid solution for later use;
(2) preparing a chitosan/mica composite material: adding mica powder with the mass ratio of 1:1 to chitosan into a chitosan acetic acid solution, stirring and fully dissolving the mica powder, transferring the mixture into an injector, then dropping the solution in the injector into a NaOH solution with the concentration of 1mol/L to form small balls, taking out the small balls after coagulation, filtering and washing the small balls to be neutral, and then drying the small balls to obtain a chitosan/mica composite material for later use;
(3) preparing a chitosan/mica/PEI composite material: taking 1mL of polyethyleneimine, adding 7mL of distilled water and 0.3mL of epoxy chloropropane, fully stirring the three to uniformly mix the mixture to obtain a soaking solution, then putting the chitosan/mica composite material into the soaking solution to soak for 4 hours, taking the chitosan/mica composite material out of the soaking solution, putting the chitosan/mica composite material into a 50 ℃ drying oven to fully react for 11 hours, then putting the drying oven into a freeze dryer to dry, and carrying out freeze drying for 24 hours at the temperature of-50 ℃ to obtain the chitosan/mica/PEI composite material.
The embodiment also provides application of the chitosan/mica/PEI composite material, including application of Se (IV) in absorption of selenious acid.
Example 2
The embodiment provides a preparation method of a chitosan/mica/PEI composite material, which comprises the following steps:
(1) preparing a chitosan acetic acid solution: weighing 0.32g of chitosan, and dissolving the chitosan in 10mL of dilute acetic acid solution with the concentration of 2% to obtain chitosan acetic acid solution for later use;
(2) preparing a chitosan/mica composite material: adding mica powder with the mass ratio of 1:2 to chitosan into a chitosan acetic acid solution, stirring and fully dissolving the mica powder, transferring the mixture into an injector, then dropping the solution in the injector into a NaOH solution with the concentration of 1mol/L to form small balls, taking out the small balls after coagulation, filtering and washing the small balls to be neutral, and then drying the small balls to obtain a chitosan/mica composite material for later use;
(3) preparing a chitosan/mica/PEI composite material: 1.5mL of polyethyleneimine is taken, 8mL of distilled water and 0.5mL of epoxy chloropropane are added, the three are fully stirred and uniformly mixed to obtain a soaking solution, then the chitosan/mica composite material is placed into the soaking solution to be soaked for 5 hours, then the chitosan/mica composite material is taken out of the soaking solution and is placed into a 55 ℃ drying oven to be fully reacted for 12 hours, then the chitosan/mica/PEI composite material is placed into a freeze drier to be dried, and the freeze drying is carried out for 24 hours at the temperature of-50 ℃ to obtain the chitosan/mica/PEI composite material.
The embodiment also provides application of the chitosan/mica/PEI composite material, including application of Se (IV) in absorption of selenious acid.
Example 3
The embodiment provides a preparation method of a chitosan/mica/PEI composite material, which comprises the following steps:
(1) preparing a chitosan acetic acid solution: weighing 0.35g of chitosan, and dissolving the chitosan in 12mL of dilute acetic acid solution with the concentration of 2% to obtain chitosan acetic acid solution for later use;
(2) preparing a chitosan/mica composite material: adding mica powder with the mass ratio of 1:4 to chitosan into a chitosan acetic acid solution, stirring and fully dissolving the mica powder, transferring the mixture into an injector, then dropping the solution in the injector into a NaOH solution with the concentration of 1mol/L to form small balls, taking out the small balls after coagulation, filtering and washing the small balls to be neutral, and then drying the small balls to obtain a chitosan/mica composite material for later use;
(3) preparing a chitosan/mica/PEI composite material: adding 9mL of distilled water and 0.7mL of epoxy chloropropane into 2mL of polyethyleneimine, fully stirring the polyethyleneimine, the distilled water and the epoxy chloropropane to uniformly mix the polyethyleneimine, the distilled water and the epoxy chloropropane to obtain a soaking solution, then putting the chitosan/mica composite material into the soaking solution to soak for 6 hours, taking the chitosan/mica composite material out of the soaking solution, putting the chitosan/mica composite material into a 60 ℃ drying oven to fully react for 13 hours, then putting the drying oven into a freeze dryer to dry, and carrying out freeze drying for 24 hours at the temperature of-50 ℃ to obtain the chitosan/mica/PEI composite material.
The embodiment also provides application of the chitosan/mica/PEI composite material, including application of Se (IV) in absorption of selenious acid.
Test and result analysis
To illustrate the utility value of the present application, the applicant also made the following tests:
a. determination of the selenium Standard Curve
Accurately measuring the selenium standard solution, and preparing the selenium standard solution with the concentration of 10mg/L by using distilled water for later use. Respectively sucking 0, 0.1, 0.5, 1.5, 2.5, 3.5, 4.5 and 5.0mL of selenium standard solution in a 25mL colorimetric tube, adding 1.0mL1.5mol/L HCl solution, heating in water bath at 40 ℃ for 20min, adding 1.0mL of 200g/L KI solution, and fixing with distilled waterShaking, measuring absorbance of the solution with ultraviolet spectrophotometer at 352nm wavelength with reagent blank as reference, and linear fitting to obtain standard Se (IV) curve equation A of 0.3136C-00.0227, R20.9997. The standard curve of Se (IV) is shown in FIG. 1.
b. Adsorption performance of composite materials with different chitosan/mica powder ratios
0.025g of chitosan/mica/PEI composite material in different ratios is respectively added into a conical flask with a plug, which is filled with 25mL of 100mg/L sodium selenite solution (except for different composition ratios of chitosan and mica powder, the other preparation methods are the preparation methods described in the embodiment 2), the pH value of the conical flask is adjusted to be 3.0, after the composite material is reacted at the constant temperature of 30 ℃, 300 mu L of supernatant is taken out and placed into a 25mL colorimetric tube every 10min, and the concentration of Se (IV) in the solution is measured according to the conditions of measuring a standard curve. After the experiment was repeated three times to obtain data, the average value was taken.
Calculating the adsorption capacity of the CxMy/PEI composite material, and testing different composite materials under the condition of ensuring the same selenium content in the solution to screen out a group of composite materials with the best adsorption capacity.
Specific ratios are shown in table 1:
TABLE 1 Chitosan/mica powder
Note: chitosan-mica Composites is abbreviated as CxMy, wherein x and y are the mass ratio of Chitosan to mica.
Results and analysis: FIG. 2 shows the effect curves of different ratios of the composite materials on Se (IV) adsorption, and it can be seen from FIG. 2 that the composite materials of C1M1/PEI and C4M1/PEI reach the adsorption equilibrium after 50min, and the equilibrium adsorption amounts are 54.2mg/g and 58.0mg/g respectively; the adsorption of the C2M1/PEI composite material in 1 hour is not balanced, the adsorption amount is increased, the adsorption amount of the C2M1/PEI is the largest relative to the adsorption amount of the C1M1/PEI and the C4M1/PEI composite material, and therefore the C2M1/PEI composite material is selected to study the adsorption capacity of Se (IV).
Influence of pH value on Se (IV) adsorption effect
0.025g of C2M1/PEI composite material with the best adsorption capacity is weighed, sequentially added with Se (IV) solutions with pH values of 3.0, 4.0, 5.0, 6.0, 7.0, 8.0, 9.0 and 10.0, wherein the initial concentrations of the eight Se (IV) solutions are respectively 100mg/L and the volumes are respectively 25.0mL, then the mixture is subjected to constant temperature reaction in a constant temperature oscillator at 30 ℃ for 2 hours, 300 mu L of supernatant is taken and put into a 25mL colorimetric tube, and the concentration of Se (IV) in the solution is measured according to the method for measuring a standard curve. After the experiment is repeated three times to obtain data, taking an average value; and the pH of the solution was determined after the experiment was completed. And calculating the adsorption quantity Qe of the composite material of C2M1/PEI at different pH values.
Note: as the composite material can be dissolved when the pH value is less than 3, the adsorption effect of the composite material on Se (IV) is greatly influenced, and the pH value is selected from 3-10 for determination.
Results and analysis: the curve of the influence of different pH values on the Se (IV) adsorption of the composite material is shown in FIG. 3, and the experimental data in FIG. 3 show that the Se (IV) adsorption effect of C2M1/PEI is better under acidic conditions; when the pH value is 3, the adsorption effect is best, and the maximum adsorption quantity is 82.6 mg/g; the adsorption effect of the C2M1/PEI composite material on Se (IV) is gradually weakened along with the increase of the pH value, and the maximum adsorption amount is about 74.0mg/g at the pH value of 9.
d. Effect of time on Se (IV) adsorption Effect
0.025g of composite material of C2M1/PEI with the best adsorption capacity and mica powder are weighed and respectively added into 25.0mL of sodium selenite solution with the pH value of 3.0 and the initial concentration of 100mg/L, constant-temperature shaking is carried out at the temperature of 30 ℃, after reaction for a certain time, 300 mu L of supernatant is taken and put into a 25mL colorimetric tube, and the concentration of Se (IV) in the solution is measured according to the condition of measuring a standard curve. After the experiment was repeated three times to obtain data, the average value was taken. And calculating the adsorption capacity of the CxMy/PEI composite material and the mica powder in different time.
Results and analysis: FIG. 4 is a graph showing the influence of different adsorption times on Se (IV) adsorption, and experimental results show that after 2 hours, the system basically reaches an adsorption equilibrium state, the adsorption capacity is not increased any more, the saturated adsorption capacities of the C2M1/PEI composite material and the mica powder are respectively about 71.7mg/g and 43.5mg/g, and the optimal adsorption time is 2 hours.
e. Influence of temperature on the adsorption Effect
0.025g of a group of C2M1/PEI composite materials with the best adsorption capacity is weighed, added into 25.0mL of sodium selenite solution with the pH value of 3.0 and the initial concentration of 100mg/L respectively, and after isothermal reaction at 20, 30, 40 and 50 ℃, 300 mu L of supernatant is taken out every 20min and put into a 25mL colorimetric tube, and the concentration of Se (IV) in the solution is measured according to the method of measuring a standard curve. And the amount of adsorption was calculated.
Results and analysis: FIG. 5 is a graph of the effect of C2M1/PEI on Se (IV) adsorption at different temperatures. Wherein the equilibrium adsorption capacity of the C2M1/PEI composite material at 20 ℃ is the minimum, and is respectively about 71.1mg/g and 72.9 mg/g; the equilibrium adsorption capacity is maximum at 50 ℃, and is respectively about 81.1mg/g and 81.8 mg/g; namely, the temperature of the external environment is raised, which is beneficial to the adsorption of the composite material on Se (IV) in the sodium selenite.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (8)
1. The chitosan/mica/PEI composite material for adsorbing Se (IV) in selenious acid is characterized in that the preparation method of the chitosan/mica/PEI composite material is as follows:
(1) preparing a chitosan acetic acid solution: weighing 0.3-0.35g of chitosan, and dissolving the chitosan in 8-12mL of dilute acetic acid solution to obtain chitosan acetic acid solution for later use;
(2) preparing a chitosan/mica composite material: adding mica powder with the mass ratio of 1:1-4 to chitosan into a chitosan acetic acid solution, stirring and fully dissolving the mica powder, transferring the mixture into an injector, then dropping the solution in the injector into a NaOH solution to form small balls, taking out the small balls after coagulation, filtering and washing the small balls to be neutral, and then drying the small balls to obtain a chitosan/mica composite material for later use;
(3) preparing a chitosan/mica/PEI composite material: taking 1-2mL of polyethyleneimine, adding 7-9mL of distilled water and 0.3-0.7mL of epoxy chloropropane, fully stirring the three to uniformly mix the mixture to obtain a soaking solution, then putting the chitosan/mica composite material into the soaking solution to soak for 4-6h, then taking the chitosan/mica composite material out of the soaking solution, putting the chitosan/mica composite material into a 50-60 ℃ drying oven to fully react for 11-13h, and then putting the drying oven into a freeze dryer to dry, thus obtaining the chitosan/mica/PEI composite material;
the mass ratio of the mica powder to the chitosan in the step (2) is 1: 2.
2. The chitosan/mica/PEI composite material for adsorbing Se (IV) in selenious acid as claimed in claim 1, wherein the amount of chitosan in the step (1) is 0.32g, and the amount of diluted acetic acid is 10 mL.
3. The chitosan/mica/PEI composite material for adsorbing Se (IV) in selenious acid as claimed in claim 1, wherein the concentration of the dilute acetic acid solution in the step (1) is 2%.
4. The chitosan/mica/PEI composite material for adsorbing Se (IV) in selenious acid as claimed in claim 1, wherein the amount of polyethyleneimine in the soaking solution in the step (3) is 1.5mL, the amount of distilled water is 8mL, and the amount of epichlorohydrin is 0.5 mL.
5. The chitosan/mica/PEI composite material for adsorbing Se (IV) in selenious acid as claimed in claim 1, wherein the concentration of the NaOH solution in the step (2) is 1 mol/L.
6. The chitosan/mica/PEI composite material for adsorbing Se (IV) in selenious acid as claimed in claim 1, wherein the freeze drying in the step (3) is drying at a temperature of-50 ℃ for 24 h.
7. The chitosan/mica/PEI composite material for adsorbing Se (IV) in selenious acid as claimed in claim 1, wherein in the step (3), the chitosan/mica composite material is placed in a soaking solution for soaking for 5 hours, and then is taken out of the soaking solution and placed in an oven at 55 ℃ to be fully reacted for 12 hours.
8. The chitosan/mica/PEI composite material for adsorbing Se (IV) in selenious acid as claimed in claim 1, wherein the adsorption conditions of the composite material applied in adsorbing selenium are as follows: the temperature is 50 ℃, the pH is 3 and the adsorption time is 2 h.
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