CN106622178A - Magnetic porous cationic polymer adsorbent and preparation method thereof - Google Patents
Magnetic porous cationic polymer adsorbent and preparation method thereof Download PDFInfo
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- CN106622178A CN106622178A CN201710056431.3A CN201710056431A CN106622178A CN 106622178 A CN106622178 A CN 106622178A CN 201710056431 A CN201710056431 A CN 201710056431A CN 106622178 A CN106622178 A CN 106622178A
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- polyethyleneimine
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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
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
- B01J20/267—Cross-linked polymers
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The invention discloses magnetic porous cationic polymer adsorbent and a preparation method thereof. The preparation method comprises the following steps of ultrasonically and evenly emulsifying ferrous chloride tetrahydrate, ferric chloride hexahydrate, polyethyleneimine and chitosan; generating ferroferric oxide nanometer particles in an in-situ nucleation mode after heating reaction, wherein the magnetic nanometer particles are included by molecular chains of the chitosan and the polyethyleneimine to form a ternary network interpenetrating composite during nucleation growth; then performing cross-linking graft on the polyethyleneimine and the composite through cross-linking reaction, so as to obtain the polyethyleneimine-chitosan magnetic porous cationic polymer adsorbent. The adsorbent has a good adsorbing effect on congo red; when the batch charge of the adsorbent is increased to 25mg, the removal rate of 100mg/L (50ml) congo red can be 95% or more; the adsorbent has a simple and quick magnetic separation function, is beneficial to simplifying a general centrifugation and settlement process which consumes time and energy in a water treatment process, and has good application prospect in the field of sewage treatment.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to a kind of attached dose of magnetic porous cation high molecular and its system
Preparation Method.
Background technology
With developing rapidly for modern industry, industrial wastewater, a large amount of discharges of family domestic waste water and agricultural chemicals, chemical fertilizer
It is unreasonable to use, the severe contamination of water body is caused, have a strong impact on the healthy living of people.Therefore, study economical and efficient
Method of wastewater treatment be current focus of concern.At present wastewater processing technology mainly have photochemical catalytic oxidation, chemical coagulation,
The technologies such as biological adsorption, wherein biological adsorption are a kind of simple, effective and methods of economy, therefore biosorption process is in Shui Chu
Reason aspect has a extensive future.Adsorbent is the key core of biological adsorption, and current adsorbent mainly has porous carbon, diatom
Soil, concave convex rod, synthetic organic polymer, agricultural wastes etc..But these adsorbents still suffer from high cost, preparation process complexity,
Using when separate inconvenient, or even the meeting having produces the deficiencies such as secondary pollution.By contrast, natural polymer base adsorbent has
Good biocompatibility and modifiability, so as to receive significant attention.
In the absorption of natural polymer subbase, shitosan is constantly subjected to the favor of people.It is distributed on chitosan molecule chain backbone
A large amount of NH2Base, OH base isopolarity groups and ionic bond, hydrogen bond etc., there is good charging neutrality and absorption to gel in water
Bridging action and shitosan is nontoxic good degradability.Polyethyleneimine is a kind of important macromolecule, as shitosan, tool
There is good biocompatibility, medicine and genophore are widely used in recent years.
The present invention prepares a kind of magnetic using Iron dichloride tetrahydrate, ferric chloride hexahydrate, polyethyleneimine and shitosan
Attached dose of porous cation macromolecule, and make possess efficient absorption property, easy Magneto separate performance and good environmental friendliness
Performance.Both polyethyleneimine pH shortcomings poor for applicability had been overcome, adsorption effect under shitosan acid, alkalescence condition had been overcome again
Difference, consumption is big, the shortcoming of high cost.
The content of the invention
Present invention aims to prior art is not enough, there is provided a kind of attached dose of magnetic porous cation high molecular and its
Preparation method, the adsorbent has efficient adsorption effect to Congo red and Cr VI, and adsorbent feeds intake increases to 25 mg pair
100 mg/L（50 mL）Congo red clearance reaches more than 95%, has a good application prospect in sewage treatment area.
For achieving the above object, the present invention is adopted the following technical scheme that：
The preparation method of attached dose of a kind of magnetic porous cation high molecular, with Iron dichloride tetrahydrate, ferric chloride hexahydrate, poly- second
Alkene imines and shitosan are base material, and Iron dichloride tetrahydrate, ferric chloride hexahydrate and shitosan ultrasonic emulsification is uniform, and heating is anti-
Should be rear in situ into karyogenesis ferriferrous oxide nano-particle, magnetic nano-particle is while nucleating growth by shitosan and poly- second
Alkene imines strand includes to form ternary network interpenetrating compound, then by cross-linking reaction, polyethyleneimine is multiple with inclusion
Compound carries out cross-linked graft, and polyethyleneimine-shitosan magnetic porous cation polymeric sorbent is obtained.
Comprise the following steps that：
（1）0.2-2.0 g Iron dichloride tetrahydrates and 0.8-6.0 g ferric chloride hexahydrates are dispersed in into 30 mL deionized waters
In, ultrasonic mixing is uniform；
（2）By step（1）The mixed solution for obtaining is added dropwise to 50 mL and has dissolved 0.5-8.0 g shitosans and 0.1-2.0g
In the acetum of polyethyleneimine, with homogenizer 15 min are emulsified；
（3）By step（2）The mixture for obtaining is transferred in there-necked flask, is passed through after nitrogen and is heated to 40-90 DEG C, adds 3-20
ML ammoniacal liquor, reacts 0.5-3.0 h, is subsequently adding 0.1-5.0 g polyethyleneimines, and with homogenizer 10 min are emulsified；
（4）Toward step（3）Epoxychloropropane 0.1-5.0 mL, cross-linking reaction 0.5-4 hour are added in the mixture for obtaining；With cold
Water terminating reaction, and adjust pH to neutrality, product freeze-drying after externally-applied magnetic field separation with 1mol/L hydrochloric acid solutions, that is, obtain
Magnetic porous cation high molecular adsorbent.
The present invention remarkable advantage be：The present invention with Iron dichloride tetrahydrate, ferric chloride hexahydrate, polyethyleneimine and
Shitosan is base material, and the method being crosslinked by the way that-inclusion in situ-is blended without soap is obtained, and the method achieves one pot process magnetic
Porous adsorbent, process is easy, realizes low energy consumption, low solvent and prepares.Obtained adsorbent of the invention waits dyestuff to Congo red
With efficient adsorption capacity, adsorbent feeds intake increases to 25 mg to 100 mg/L（50 mL）Congo red clearance reaches
More than 95%, and with simple, efficiently Magneto separate function, be conducive to simplifying commonly use in water treatment procedure time-consuming, power consumption
Centrifugation, infall process, have a good application prospect in sewage treatment area.
Description of the drawings
Fig. 1 is the SEM figures of magnetic porous cation high molecular adsorbent；
Fig. 2 is magnetic porous cation high molecular adsorbent to Congo red the adsorption effect figure.
Specific embodiment
Embodiment 1：
（1）0.2 g Iron dichloride tetrahydrates and 0.8 g ferric chloride hexahydrates are dispersed in 30 mL deionized waters, ultrasound is mixed
Close uniform；
（2）By step（1）The mixed solution for obtaining is added dropwise to 50 mL and has dissolved 0.5 g shitosans and 0.1g polyethyleneimines
In the acetum of amine, with homogenizer 15 min are emulsified；
（3）By step（2）The mixture for obtaining is transferred in there-necked flask, is passed through after nitrogen and is heated to 40 DEG C, adds 3 mL ammonia
Water, reacts 0.5 h, is subsequently adding 0.1 g polyethyleneimines, and with homogenizer 10 min are emulsified；
（4）Toward step（3）The mL of epoxychloropropane 0.1, cross-linking reaction 0.5 hour are added in the mixture for obtaining；Terminated with cold water
Reaction, and adjust pH to neutrality, product freeze-drying after externally-applied magnetic field separation with 1mol/L hydrochloric acid solutions, that is, obtain magnetic many
Hole cation high molecular adsorbent；
（5）2.5 mg adsorbents are added in the Congo red solution of 50 mL, in the h of ultrasonic wave stirring and adsorbing 3, mensuration absorbance,
Detection adsorption effect.
Embodiment 2：
（1）0.5 g Iron dichloride tetrahydrates and 2.5 g ferric chloride hexahydrates are dispersed in 30 mL deionized waters, ultrasound is mixed
Close uniform；
（2）By step（1）The mixed solution for obtaining is added dropwise to 50 mL and has dissolved 1.0 g shitosans and 0.3g polyethyleneimines
In the acetum of amine, with homogenizer 15 min are emulsified；
（3）By step（2）The mixture for obtaining is transferred in there-necked flask, is passed through after nitrogen and is heated to 80 DEG C, adds 5.0 mL
Ammoniacal liquor, reacts 1.5 h, is subsequently adding 0.8 g polyethyleneimines, and with homogenizer 10 min are emulsified；
（4）Toward step（3）The mL of epoxychloropropane 0.4, cross-linking reaction 1.0 hours are added in the mixture for obtaining；Terminated with cold water
Reaction, and adjust pH to neutrality, product freeze-drying after externally-applied magnetic field separation with 1mol/L hydrochloric acid solutions, that is, obtain magnetic many
Hole cation high molecular adsorbent；
（5）10 mg adsorbents are added in the Congo red solution of 50 mL, in the h of ultrasonic wave stirring and adsorbing 3, mensuration absorbance, inspection
Survey adsorption effect.
Embodiment 3：
（1）1.0 g Iron dichloride tetrahydrates and 2.5 g ferric chloride hexahydrates are dispersed in 30 mL deionized waters, ultrasound is mixed
Close uniform；
（2）By step（1）The mixed solution for obtaining is added dropwise to 50 mL and has dissolved 1.2 g shitosans and 1.0g polyethyleneimines
In the acetum of amine, with homogenizer 15 min are emulsified.
（3）By step（2）The mixture for obtaining is transferred in there-necked flask, is passed through after nitrogen and is heated to 90 DEG C, is added
11.0 mL ammoniacal liquor, react 1.0 h, are subsequently adding 2.0 g polyethyleneimines, and with homogenizer 10 min are emulsified；
（4）Toward step（3）The mL of epoxychloropropane 1.0, cross-linking reaction 2.0 hours are added in the mixture for obtaining；Terminated with cold water
Reaction, and adjust pH to neutrality, product freeze-drying after externally-applied magnetic field separation with 1mol/L hydrochloric acid solutions, that is, obtain magnetic many
Hole cation high molecular adsorbent；
（5）25 mg adsorbents are added in the Congo red solution of 50 mL, in the h of ultrasonic wave stirring and adsorbing 3, mensuration absorbance, inspection
Survey adsorption effect.
Embodiment 4：
（1）1.5 g Iron dichloride tetrahydrates and 4.0 g ferric chloride hexahydrates are dispersed in 30 mL deionized waters, ultrasound is mixed
Close uniform；
（2）By step（1）The mixed solution for obtaining is added dropwise to 50 mL and has dissolved 2.0 g shitosans and 1.5g polyethyleneimines
In the acetum of amine, with homogenizer 15 min are emulsified；
（3）By step（2）The mixture for obtaining is transferred in there-necked flask, is passed through after nitrogen and is heated to 90 DEG C, adds 20 mL ammonia
Water, reacts 1.5 h, is subsequently adding 3.0 g polyethyleneimines, and with homogenizer 10 min are emulsified；
（4）Toward step（3）The mL of epoxychloropropane 3.0, cross-linking reaction 3.0 hours are added in the mixture for obtaining；Terminated with cold water
Reaction, and adjust pH to neutrality, product freeze-drying after externally-applied magnetic field separation with 1mol/L hydrochloric acid solutions, that is, obtain magnetic many
Hole cation high molecular adsorbent；
（5）50 mg adsorbents are added in the Congo red solution of 50 mL, in the h of ultrasonic wave stirring and adsorbing 3, mensuration absorbance, inspection
Survey adsorption effect.
Embodiment 5：
（1）2.0 g Iron dichloride tetrahydrates and 6.0 g ferric chloride hexahydrates are dispersed in 30 mL deionized waters, ultrasound is mixed
Close uniform；
（2）By step（1）The mixed solution for obtaining is added dropwise to 50 mL and has dissolved 3.0 g shitosans and 2.0g polyethyleneimines
In the acetum of amine, with homogenizer 15 min are emulsified；
（3）By step（2）The mixture for obtaining is transferred in there-necked flask, is passed through after nitrogen and is heated to 65 DEG C, adds 12 mL ammonia
Water, reacts 3.0 h, is subsequently adding 1.0 g polyethyleneimines, and with homogenizer 10 min are emulsified；
（4）Toward step（3）The mL of epoxychloropropane 5.0, cross-linking reaction 4.0 hours are added in the mixture for obtaining；Terminated with cold water
Reaction, and adjust pH to neutrality, product freeze-drying after externally-applied magnetic field separation with 1mol/L hydrochloric acid solutions, that is, obtain magnetic many
Hole cation high molecular adsorbent；
（5）70 mg adsorbents are added in the Congo red solution of 50 mL, in the h of ultrasonic wave stirring and adsorbing 3, mensuration absorbance, inspection
Survey adsorption effect.
From figure 1 it appears that the adsorbent surface not only surface is more coarse, it is uneven to have many folds concurrently, and
Porous network structure is defined by cross-linking reaction between each strand, this structure can provide very big specific surface and activity
Adsorption site, so as to high performance adsorption capacity.
From figure 2 it can be seen that the adsorbent feeds intake increases to 25 mg to 100 mg/L（50 mL）Congo red removal
Rate reaches more than 95%, illustrates the adsorbent to Congo red with good Adsorption effect.
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent with
Modification, should all belong to the covering scope of the present invention.
Claims (3)
1. a kind of magnetic porous cation high molecular adsorbent, it is characterised in that：The adsorbent be with Iron dichloride tetrahydrate, six
Ferric Chloride Hydrated, polyethyleneimine and shitosan are base material, many obtained in the method that-inclusion in situ-is crosslinked by being blended without soap
Hole magnetic high-efficiency adsorbent.
2. a kind of method for preparing magnetic porous cation high molecular adsorbent as claimed in claim 1, it is characterised in that：Will
Iron dichloride tetrahydrate, ferric chloride hexahydrate, polyethyleneimine and shitosan ultrasonic emulsification are uniform, nucleation in situ after heating response
Ferriferrous oxide nano-particle is generated, magnetic nano-particle is while nucleating growth by shitosan and polyethyleneimine strand
Inclusion forms ternary network interpenetrating compound, and then by cross-linking reaction, by polyethyleneimine, further crosslinking connects with compound
Branch, is obtained polyethyleneimine-shitosan magnetic porous cation polymeric sorbent.
3. the preparation method of magnetic porous cation high molecular adsorbent according to claim 2, it is characterised in that：Specifically
Step is as follows：
（1）0.2-2.0 g Iron dichloride tetrahydrates and 0.8-6.0 g ferric chloride hexahydrates are dispersed in into 30 mL deionized waters
In, ultrasonic mixing is uniform；
（2）By step（1）The mixed solution for obtaining is added dropwise to 50 mL and has dissolved 0.5-8.0 g shitosans and 0.1-2.0g
In the acetum of polyethyleneimine, with homogenizer 15 min are emulsified；
（3）By step（2）The mixture for obtaining is transferred in there-necked flask, is passed through after nitrogen and is heated to 40-90 DEG C, adds 3-20
ML ammoniacal liquor, reacts 0.5-3.0 h, is subsequently adding 0.1-5.0 g polyethyleneimines, and with homogenizer 10 min are emulsified；
（4）Toward step（3）Epoxychloropropane 0.1-5.0 mL, cross-linking reaction 0.5-4 hour are added in the mixture for obtaining；Use water
Terminating reaction, and adjust pH to neutrality, product freeze-drying after externally-applied magnetic field separation with 1mol/L hydrochloric acid solutions, that is, obtain magnetic
Property porous cation polymeric sorbent.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109250724A (en) * | 2017-07-14 | 2019-01-22 | 中国地质大学（北京） | Attapulgite@ferroso-ferric oxide one-dimensional magnetic nanocomposite and preparation method thereof |
| CN110193360A (en) * | 2019-06-28 | 2019-09-03 | 厦门德露滋环保科技有限公司 | A kind of induction crystallisation material for water treatment and preparation method thereof |
| CN112090406A (en) * | 2020-08-24 | 2020-12-18 | 兰州理工大学 | Preparation method of polyethyleneimine modified chitosan magnetic composite material |
| CN112574983A (en) * | 2021-01-08 | 2021-03-30 | 福州大学 | Preparation method and application of recyclable immobilized enzyme |
| CN113952939A (en) * | 2020-07-21 | 2022-01-21 | 天津大学 | Preparation method and application of amino modified ferrihydrite material |
| CN114749158A (en) * | 2022-03-18 | 2022-07-15 | 华南理工大学 | Polyethyleneimine/chitosan composite adsorbent as well as preparation method and application thereof |
| CN115337912A (en) * | 2022-08-03 | 2022-11-15 | 河池学院 | Magnetic cross-linked chitosan-polyethyleneimine/biochar composite gel particles and preparation method thereof |
| CN115445581A (en) * | 2022-09-09 | 2022-12-09 | 河池学院 | pH-responsive amphipathic sodium alginate-embedded magnetic chitosan-polyethyleneimine hydrogel and preparation method thereof |
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| CN109529780B (en) * | 2018-11-19 | 2021-07-27 | 福州大学 | Magnetic porous adsorbent and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109250724A (en) * | 2017-07-14 | 2019-01-22 | 中国地质大学（北京） | Attapulgite@ferroso-ferric oxide one-dimensional magnetic nanocomposite and preparation method thereof |
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| CN114749158A (en) * | 2022-03-18 | 2022-07-15 | 华南理工大学 | Polyethyleneimine/chitosan composite adsorbent as well as preparation method and application thereof |
| CN115337912A (en) * | 2022-08-03 | 2022-11-15 | 河池学院 | Magnetic cross-linked chitosan-polyethyleneimine/biochar composite gel particles and preparation method thereof |
| CN115445581A (en) * | 2022-09-09 | 2022-12-09 | 河池学院 | pH-responsive amphipathic sodium alginate-embedded magnetic chitosan-polyethyleneimine hydrogel and preparation method thereof |
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| CN106622178B (en) | 2019-06-07 |
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