CN110523399A - A kind of preparation method and applications of chitosan/mica/PEI composite material - Google Patents
A kind of preparation method and applications of chitosan/mica/PEI composite material Download PDFInfo
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- CN110523399A CN110523399A CN201910859040.4A CN201910859040A CN110523399A CN 110523399 A CN110523399 A CN 110523399A CN 201910859040 A CN201910859040 A CN 201910859040A CN 110523399 A CN110523399 A CN 110523399A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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 present invention provides a kind of preparation method of chitosan/mica/PEI composite material, it is related to technical field of composite preparation, the preparation process of chitosan/mica/PEI composite material preparation method of the invention is the following steps are included: (1) prepares chitosan acetic acid solution, (2) prepare chitosan/mica composite material, (3) prepare chitosan/mica/PEI composite material；The present invention is using chitosan/acetic acid regenerated composite material as research object, chitosan/mica modified composite material is prepared for by physical blending method, then it is reacted using epoxychloropropane as crosslinking agent with polyethyleneimine and prepares novel chitosan/mica/PEI composite organic-inorganic material, and it is applied to the Se (IV) in absorption selenous acid, recycling is collected to Se (IV) excessive in water body, the dangerous problem that not only can solve selenium can be used as controlled release selenium fertilizer by processing appropriate.
Description
[technical field]
The present invention relates to technical field of composite preparation, and in particular to a kind of chitosan/mica/PEI composite material
Preparation method and applications.
[background technique]
Selenium (Selenium, Se) is a kind of teleorganic microelement, is selenocysteine and selenoenzyme such as peroxide
The required component of compound enzyme, anticancer, in terms of play a significant role.Research finds that application selenium can resist plant
Interior free radical injury, the growth and development for promoting plant, while it being also act against heavy metal, improve the resistance of plant.Not similar shape
State selenium has facilitation to aquatile growth and development as feed addictive, and immunity of organisms and inoxidizability can be improved.
But selenous acid and its salt have very strong bio-toxicity, and the spies such as its water-soluble strong, easy loss.With selenium
Extensive use in electronics industry, agricultural, because of its improper use, excessive emissions, it will cause serious dirt to ecological environment
Dye.Currently, absorption method because its is easy to operate, good separating effect, is the removal master for selenous acid in water body and its salt Se (IV)
Want one of method.And it is adsorbed on the selenium source in degradation material and can be used as the nutritional agents lacked in selenium soil, or be used for selenium
The additive in source.Therefore, recycling is collected to Se (IV) excessive in water body using absorption method, not only can solve selenium
Dangerous problem can be used as selenium fertilizer by processing appropriate.
Contain a large amount of amido and carboxyl in the molecular structure of chitosan, therefore it also has absorption well to make to heavy metal
With however, since its mechanical performance is weak, being easy degradation and unstable in acid condition, and it is using also restrained.It is logical
Amido and hydroxyl in chemical reaction modification chitosan molecule chain are crossed, modification of chitosan is obtained, since the orphan on imido nitrogen atom is right
Electronics has good nucleophilicity, so the research for carrying out amido chemical modification to chitosan molecule is relatively more.
But as adsorbent material for, above-mentioned these are modified the promotion of the absorption property of unfavorable chitosan instead.Firstly,
By amido reaction modifying chitosan, the quantity of amino that can be quaternized is not only reduced, so that the reduction of adsorption capacity, and
With water-soluble increase, material is separated from water body after being unfavorable for absorption.
As natural high molecular substance, the absorption property of chitosan is again by its own physical aspect, deacetylation and body
It is the influence of pH value.Therefore, physics is carried out to it and chemical modification be improve chitosan absorption property, expand application range must
Want means.Currently, chitosan is compounded in for absorbing heavy metal ions using more, technology is more mature, but it is used for pair
The research of Se (IV) absorption property is rarely reported.
It can be seen that researching and developing suitable Se (IV) adsorbent, to prevention, its is potentially hazardous and is collected recycling
With positive meaning.
[summary of the invention]
In view of this, the purpose of the present invention is to provide a kind of preparation method of chitosan/mica/PEI composite material, this
Invention is prepared for chitosan/mica using chitosan/acetic acid regenerated composite material as research object, by physical blending method
Modified composite material, then reacted using epoxychloropropane as crosslinking agent with polyethyleneimine prepare novel chitosan/mica/
PEI composite organic-inorganic material.
In order to solve the above-mentioned technical problem, present invention employs the following technical solutions:
A kind of preparation method of chitosan/mica/PEI composite material, steps are as follows:
(1) it prepares chitosan acetic acid solution: weighing the chitosan of 0.3-0.35g, be dissolved in the acetic acid diluted of 8-12mL
In solution, chitosan acetic acid solution is obtained, it is spare；
(2) prepare chitosan/mica composite material: in chitosan acetic acid solution, being added with chitosan mass ratio is 1:
The mica powder of 1-4 is stirred for after completely dissolution, being transferred in syringe, and it is molten that the solution in syringe is then instilled NaOH
In liquid, bead is formed, is taken out after condensing, is filtered and wash to neutrality, be then dried, it is compound to obtain chitosan/mica
Material, it is spare；
(3) prepare chitosan/mica/PEI composite material: taking 1-2mL polyethyleneimine, be added 7-9mL distilled water and
0.3-0.7mL epoxychloropropane, three, which is sufficiently stirred, which is uniformly mixed it, obtains soak, then that chitosan/mica is multiple
Condensation material, which is put into soak, impregnates 4-6h, it is then put into 50-60 DEG C of baking oven after taking out in soak keeps it sufficiently anti-
11-13h is answered, drying in freeze drier is then placed in, chitosan/mica/PEI composite material can be obtained.
In the present invention, further, the amount of chitosan is preferably 0.32g in the step (1), and the amount of acetic acid diluted is preferably
10mL。
In the present invention, further, the mass ratio of mica powder and chitosan is preferably 1:2 in the step (2).
In the present invention, further, the concentration of dilute acetic acid solutions is 2% in the step (1).
In the present invention, further, the amount of polyethyleneimine is preferably 1.5mL in the soak of the step (3), distillation
The amount of water is preferably 8mL, and the amount of epoxychloropropane is preferably 0.5mL.
In the present invention, further, the concentration of NaOH solution is 1mol/L in the step (2).
In the present invention, further, freeze-drying is dry under conditions of temperature is -50 DEG C in the step (3)
24h。
In the present invention, further, chitosan/mica composite material is put into soak in the step (3) and is impregnated
Time is 5h, it, which is then put into 55 DEG C of baking ovens after taking out in soak, makes it sufficiently react 12h.
The present invention also provides the applications of above-mentioned chitosan/mica/PEI composite material, including the Se in absorption selenous acid
(IV) application obtains absorption optimum condition by a large number of experiments research are as follows: temperature is 50 DEG C, pH 3, adsorption time 2h.
In conclusion by adopting the above-described technical solution, the present invention is include at least the following beneficial effects:
1. the technological process of production of the invention is short, operating condition is simple, and preparation process is completed by easy steps, is produced into
This is low, and required equipment is simple, it is easy to accomplish large-scale production.
2. the present invention passes through easy physical blending side using chitosan/acetic acid regenerated composite material as research object
Method is prepared for chitosan/mica modified composite material, then using epoxychloropropane as crosslinking agent and polyethyleneimine
Novel chitosan/mica/PEI composite organic-inorganic material is prepared in (Polyethyleneimine, PEI) reaction, and will
It is applied to the Se (IV) in absorption selenous acid, is collected recycling to Se (IV) excessive in water body, not only can solve
The dangerous problem of selenium can be used as selenium fertilizer by processing appropriate；The optimal ratio of components of adsorption effect is obtained by test of many times
Example；Then by studying influence of each factor to Se (IV) adsorption capacity using experiment of single factor.Obtain C2M1/PEI composite wood
The adsorption capacity of material is best, and when initial concentration is 100mg/L, pH=3, adsorption time 2h, temperature are 50 DEG C, C2M1/PEI is multiple
Condensation material adsorption equilibrium capacity is best, the removal rate highest of Se (IV).The application is based on chitosan-mica composite material absorption
The research of Se (IV) and practice principle establish certain basis in solution, have substantive distinguishing features outstanding and significant progress.
[Detailed description of the invention]
Fig. 1 is Se (IV) canonical plotting
Fig. 2 is the influence curve figure that the composite material of different chitosan ratios adsorbs Se (IV)；
Fig. 3 is the influence curve figure that different pH value adsorb composite material Se (IV)；
Fig. 4 be after mica and Optimal Ratio under trielement composite material C2M1/PEI to the influence curve figure of Se (IV) absorption；
Fig. 5 is the influence curve figure that C2M1/PEI adsorbs Se (IV) under different temperatures.
Test and interpretation of result are shown in attached drawing analysis.
[specific embodiment]
The following examples can help those skilled in the art that the present invention is more fully understood, but cannot be with any
Mode limits the present invention.
Embodiment 1
The present embodiment provides a kind of preparation methods of chitosan/mica/PEI composite material, comprising the following steps:
(1) it prepares chitosan acetic acid solution: weighing the chitosan of 0.3g, be dissolved in 8mL, dilute second that concentration is 2%
In acid solution, chitosan acetic acid solution is obtained, it is spare；
(2) prepare chitosan/mica composite material: in chitosan acetic acid solution, being added with chitosan mass ratio is 1:1
Mica powder, be stirred for after completely dissolution, being transferred in syringe, then by syringe solution instill concentration be
In the NaOH solution of 1mol/L, bead is formed, is taken out after condensing, is filtered and wash to neutrality, be then dried, obtain shell
Glycan/mica composite material, it is spare；
(3) it prepares chitosan/mica/PEI composite material: taking 1mL polyethyleneimine, 7mL distilled water and 0.3mL ring is added
Oxygen chloropropane, three, which is sufficiently stirred, which is uniformly mixed it, obtains soak, and chitosan/mica composite material is then put into leaching
4h is impregnated in bubble liquid, it, which is then put into 50 DEG C of baking ovens after taking out in soak, makes it sufficiently react 11h, is then placed in freezing
Dry in drying machine, freeze-drying is that for 24 hours, it is multiple that chitosan/mica/PEI can be obtained in drying under conditions of temperature is -50 DEG C
Condensation material.
The present embodiment also provides the application of above-mentioned chitosan/mica/PEI composite material, including in absorption selenous acid
The application of Se (IV).
Embodiment 2
The present embodiment provides a kind of preparation methods of chitosan/mica/PEI composite material, comprising the following steps:
(1) prepare chitosan acetic acid solution: weighing the chitosan of 0.32g, be dissolved in 10mL, concentration be 2% it is dilute
In acetic acid solution, chitosan acetic acid solution is obtained, it is spare；
(2) prepare chitosan/mica composite material: in chitosan acetic acid solution, being added with chitosan mass ratio is 1:2
Mica powder, be stirred for after completely dissolution, being transferred in syringe, then by syringe solution instill concentration be
In the NaOH solution of 1mol/L, bead is formed, is taken out after condensing, is filtered and wash to neutrality, be then dried, obtain shell
Glycan/mica composite material, it is spare；
(3) it prepares chitosan/mica/PEI composite material: taking 1.5mL polyethyleneimine, 8mL distilled water and 0.5mL is added
Epoxychloropropane, three, which is sufficiently stirred, which is uniformly mixed it, obtains soak, is then put into chitosan/mica composite material
5h is impregnated in soak, it, which is then put into 55 DEG C of baking ovens after taking out in soak, makes it sufficiently react 12h, is then placed in cold
Dry in lyophilizer, freeze-drying is that for 24 hours, chitosan/mica/PEI can be obtained in drying under conditions of temperature is -50 DEG C
Composite material.
The present embodiment also provides the application of above-mentioned chitosan/mica/PEI composite material, including in absorption selenous acid
The application of Se (IV).
Embodiment 3
The present embodiment provides a kind of preparation methods of chitosan/mica/PEI composite material, comprising the following steps:
(1) prepare chitosan acetic acid solution: weighing the chitosan of 0.35g, be dissolved in 12mL, concentration be 2% it is dilute
In acetic acid solution, chitosan acetic acid solution is obtained, it is spare；
(2) prepare chitosan/mica composite material: in chitosan acetic acid solution, being added with chitosan mass ratio is 1:4
Mica powder, be stirred for after completely dissolution, being transferred in syringe, then by syringe solution instill concentration be
In the NaOH solution of 1mol/L, bead is formed, is taken out after condensing, is filtered and wash to neutrality, be then dried, obtain shell
Glycan/mica composite material, it is spare；
(3) it prepares chitosan/mica/PEI composite material: taking 2mL polyethyleneimine, 9mL distilled water and 0.7mL ring is added
Oxygen chloropropane, three, which is sufficiently stirred, which is uniformly mixed it, obtains soak, and chitosan/mica composite material is then put into leaching
6h is impregnated in bubble liquid, it, which is then put into 60 DEG C of baking ovens after taking out in soak, makes it sufficiently react 13h, is then placed in freezing
Dry in drying machine, freeze-drying is that for 24 hours, it is multiple that chitosan/mica/PEI can be obtained in drying under conditions of temperature is -50 DEG C
Condensation material.
The present embodiment also provides the application of above-mentioned chitosan/mica/PEI composite material, including in absorption selenous acid
The application of Se (IV).
Test and interpretation of result
In order to illustrate the practical value of the application, applicant has also done following tests:
A. the measurement of selenium standard curve
It is accurate to measure selenium standard solution, the selenium Standard Stock solutions that concentration is 10mg/L are made into distilled water, it is spare.In
In 25mL colorimetric cylinder, 0,0.1,0.5,1.5,2.5,3.5,4.5,5.0mL selenium standard solution are drawn respectively, are added
200g/L KI solution 1.0mL is added in 1.0mL1.5mol/L HCl solution after 40 DEG C of heating water bath 20min, fixed with distilled water
Appearance shakes up, and using reagent blank as reference, with the absorbance value of ultraviolet specrophotometer measurement solution at 352nm wavelength, goes forward side by side
Row linear fit obtains Se (IV) calibration curve equation A=0.3136C-00.0227, R2=0.9997.Se (IV) standard curve
As shown in Figure 1.
B. the absorption property of different chitosan/mica powder ratio composite materials
Chitosan/mica/PEI composite material of 0.025g difference ratio is taken to be added to equipped with 25mL 100mg/L's respectively
(other than chitosan, mica powder composition ratio are different, other make the composite material in the stuffed conical flask of sodium selenite solution
Preparation Method is preparation method as described in example 2), adjusting its pH is 3.0, after 30 DEG C of isothermal reactions, is taken after 10min
300 μ L of clear liquid is placed in 25mL colorimetric cylinder, and the concentration of Se in solution (IV) is measured according to the condition of mark directrix curve.Experiment repeats
After obtaining data three times, it is averaged.
The adsorbance for calculating CxMy/PEI composite material, Se content is under the same conditions, multiple to difference in guaranteeing solution
Condensation material is tested, to filter out the best one group of composite material of adsorption capacity.
Specific ratio is as shown in table 1:
1 chitosan of table/mica powder
Note: Chitosan-mica Composites is abbreviated as CxMy, wherein x, and y is the mass ratio of chitosan and mica.
As a result from analysis: the influence curve that the composite material of different ratios adsorbs Se (IV) is as shown in Fig. 2, according to fig. 2
It is found that the composite material of C1M1/PEI and C4M1/PEI reaches adsorption equilibrium after 50min, equilibrium adsorption capacity is respectively
54.2mg/g with 58.0mg/g；And C2M1/PEI composite material is adsorbed in 1h and is also not up to balanced, adsorbance is also increasing, phase
For the adsorbance of C1M1/PEI and C4M1/PEI composite material, the adsorbance of C2M1/PEI is maximum, therefore selects C2M1/
The composite material of PEI studies the adsorption capacity to Se (IV).
Influence of the c.pH value to Se (IV) adsorption effect
The composite material for weighing the best C2M1/PEI of 0.025g adsorption capacity, sequentially add pH=3.0,4.0,5.0,
6.0, in 7.0,8.0,9.0,10.0 Se (IV) solution, eight groups of Se (IV) initial concentration solutions are respectively 100mg/L, volume point
Other 25.0mL then in 30 DEG C of constant temperature oscillator after isothermal reaction 2h, takes 300 μ L of supernatant to be put into 25mL colorimetric cylinder,
The concentration of Se in solution (IV) is measured according to the method for mark directrix curve.After experiment obtains data in triplicate, it is averaged；And
Solution ph is measured after the end of the experiment.Calculate adsorbance Qe of the composite material of C2M1/PEI at different pH.
Note: since composite material can be dissolved in pH < 3, extreme influence composite material to the adsorption effect of Se (IV),
Therefore pH chooses 3-10 to measure.
As a result from analysis: different pH value are to composite material Se (IV) influence curve adsorbed as shown in figure 3, from the reality of Fig. 3
Test statistics indicate that, C2M1/PEI is preferable to the adsorption effect of Se (IV) in acid condition；When pH is 3, adsorption effect is best, most
Big adsorbance is 82.6mg/g；With the increase of pH, C2M1/PEI composite material gradually weakens the suction-operated of Se (IV), In
When pH is 9, maximal absorptive capacity is in 74.0mg/g or so.
D. influence of the time to Se (IV) adsorption effect
The composite material and mica powder for weighing one group of best C2M1/PEI of 0.025g adsorption capacity are added separately to
25.0mL, pH=3.0, initial concentration are under conditions of 30 DEG C, to carry out isothermal vibration in the sodium selenite solution of 100mg/L,
After reacting the regular hour, takes 300 μ L of supernatant to be put into 25mL colorimetric cylinder, measured in solution according to the condition of mark directrix curve
The concentration of Se (IV).After experiment obtains data in triplicate, its average value is taken.And calculate CxMy/PEI composite material, mica powder
Adsorbance under different time.
As a result and analyze: Fig. 4 is the influence curve figure adsorbed under different adsorption times to Se (IV), the experimental results showed that,
System basically reaches adsorption equilibrium state after 2h, and adsorbance is not further added by, the saturation of C2M1/PEI composite material and mica powder
Adsorbance show that the optimal adsorption time is 2h respectively in 71.7mg/g, 43.5mg/g or so.
E. influence of the temperature to adsorption effect
The composite material for weighing one group of best C2M1/PEI of 0.025g adsorption capacity, is added separately to be equipped with wherein
25.0mL, pH=3.0, initial concentration are in the sodium selenite solution of 100mg/L, and constant temperature is anti-in 20,30,40,50 DEG C respectively
Ying Hou takes 300 μ L of supernatant to be put into 25mL colorimetric cylinder, measures Se in solution according to the method for mark directrix curve every 20min
(IV) concentration.And calculate its adsorbance.
As a result and analyze: Fig. 5 is the influence curve that C2M1/PEI adsorbs Se (IV) under different temperatures.Wherein C2M1/PEI
Composite material equilibrium adsorption capacity at 20 DEG C is minimum, respectively in 71.1mg/g, 72.9mg/g or so；Equilibrium adsorption capacity is most at 50 DEG C
Greatly, respectively in 81.1mg/g, 81.8mg/g or so；Ambient temperature is increased, is conducive to composite material in sodium selenite
The absorption of Se (IV).
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, fall within the scope of the claimed invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. a kind of preparation method of chitosan/mica/PEI composite material, which is characterized in that it is described the preparation method is as follows:
(1) it prepares chitosan acetic acid solution: weighing the chitosan of 0.3-0.35g, be dissolved in the dilute acetic acid solutions of 8-12mL
In, chitosan acetic acid solution is obtained, it is spare；
(2) it prepares chitosan/mica composite material: in chitosan acetic acid solution, being added and chitosan mass is than for 1:1-4's
Mica powder is stirred for after completely dissolution, being transferred in syringe, then instills the solution in syringe in NaOH solution,
Bead is formed, is taken out after condensing, is filtered and wash to neutrality, be then dried, obtain chitosan/mica composite material,
It is spare；
(3) it prepares chitosan/mica/PEI composite material: taking 1-2mL polyethyleneimine, 7-9mL distilled water and 0.3- is added
0.7mL epoxychloropropane, three, which is sufficiently stirred, which is uniformly mixed it, obtains soak, then by chitosan/mica composite wood
Material, which is put into soak, impregnates 4-6h, it, which is then put into 50-60 DEG C of baking oven after taking out in soak, makes it sufficiently react 11-
13h is then placed in drying in freeze drier, chitosan/mica/PEI composite material can be obtained.
2. a kind of preparation method of chitosan/mica/PEI composite material according to claim 1, which is characterized in that institute
The amount for stating chitosan in step (1) is preferably 0.32g, and the amount of acetic acid diluted is preferably 10mL.
3. a kind of preparation method of chitosan/mica/PEI composite material according to claim 1, which is characterized in that institute
Stating the mass ratio of mica powder and chitosan in step (2) is preferably 1:2.
4. a kind of preparation method of chitosan/mica/PEI composite material according to claim 1, which is characterized in that institute
The concentration for stating dilute acetic acid solutions in step (1) is 2%.
5. a kind of preparation method of chitosan/mica/PEI composite material according to claim 1, which is characterized in that institute
The amount for stating polyethyleneimine in the soak of step (3) is preferably 1.5mL, and the amount of distilled water is preferably 8mL, epoxychloropropane
Amount is preferably 0.5mL.
6. a kind of preparation method of chitosan/mica/PEI composite material according to claim 1, which is characterized in that institute
The concentration for stating NaOH solution in step (2) is 1mol/L.
7. a kind of preparation method of chitosan/mica/PEI composite material according to claim 1, which is characterized in that institute
Stating freeze-drying in step (3) is dried for 24 hours under conditions of temperature is -50 DEG C.
8. a kind of preparation method of chitosan/mica/PEI composite material according to claim 1, which is characterized in that institute
Stating and chitosan/mica composite material is put into soaking time in soak in step (3) is 5h, then takes it from soak
55 DEG C of baking ovens are put into after out makes it sufficiently react 12h.
9. a kind of chitosan/mica/PEI composite material according to claim 1-8 is in absorption selenous acid
The application of Se (IV).
10. application according to claim 9, which is characterized in that the chitosan/mica/PEI composite material is being applied to
Adsorb the adsorption conditions in selenium are as follows: temperature is 50 DEG C, pH 3, adsorption time 2h.
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| CN114669199A (en) * | 2022-03-15 | 2022-06-28 | 山东大学 | Modified mica sheet-nanocellulose composite nanofiltration membrane and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114669199A (en) * | 2022-03-15 | 2022-06-28 | 山东大学 | Modified mica sheet-nanocellulose composite nanofiltration membrane and preparation method thereof |
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