CN106345432B - A kind of preparation method of polyacrylamide modified magnetic loofah adsorbent - Google Patents
A kind of preparation method of polyacrylamide modified magnetic loofah adsorbent Download PDFInfo
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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
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- 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
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses a kind of preparation method of polyacrylamide modified magnetic loofah adsorbent, it is characterised in that first, in the reactor, is added by following composition mass percentage concentration, deionized water：75 ~ 82%, ferric ion：2.5 ~ 6%, ferrous ion：1.5 ~ 3%, divalent cobalt ion：0.5 ~ 2%, Aerosol OT：0.5 ~ 1.5%, after ultrasonic dissolution, add pretreatment luffa：10 ~ 15%, pH is between 11 ~ 13 for regulation, and temperature rises to 120 ± 2 DEG C of 10 ~ 12h of isothermal reaction, separation of solid and liquid, washs, and dries, obtains magnetic luffa；Then, in the reactor, added by following composition mass percentage concentration, deionized water：72 ~ 78%, polyacrylamide：4 ~ 10%, magnetic luffa：15 ~ 20%, separation of solid and liquid, wash, dry, obtain polyacrylamide modified magnetic loofah adsorbent.The adsorbent has very high adsorption capacity to perfluoro caprylic acid, and not only cost was low but also green, high mechanical strength, can Reusability more than 10 times, adsorbent can be easily separated.
Description
Technical field
The present invention relates to a kind of technical field of the preparation method of biological adsorption agent, more particularly to a kind of polyacrylamide changes
Property magnetic loofah adsorbent preparation method and to perfluoro caprylic acid (PFOA) absorption application technology, belong to regenerated resourcesization profit
With and environment and technical field of chemistry.
Background technology
In water treatment procedure, adsorbent passes through the various active groups in surface in addition using its abundant structure, specific surface area
Group and the interaction of adsorbate, extract pollutant, so as to have the function that purification of water quality from liquid phase.Wherein, absorption method
Compared with other techniques advantage be to handle the reluctant metal ion of bioanalysis, hardly degraded organic substance and some it is cloudy from
Sub- pollutant.But at the same time, for absorption method there is also many weak points, it is always to hinder that wherein the separation of solid and liquid of adsorbent is difficult
Hinder a big problem of adsorption technology progress, thus many scholars are directed to studying magnetic adsorbent and applied in water body in recent years
The removal of polluter.Research understands that with the help of externally-applied magnetic field, magnetic adsorbent can quickly realize separation of solid and liquid, and
Possess the mass transfer rate of high speed and good contacting efficiency simultaneously, thus can largely solve traditional absorption method institute
Problems faced.
Perfluoro caprylic acid（PFOA）, or it is referred to as " C8 ", it is a kind of artificial synthesized chemicals, is typically used to produce efficiently
Indispensable processing aid during energy fluoropolymer.These high-effect fluoropolymers can be widely used in Aero-Space section
Skill, transport, electronics industry, and kitchen tools（Such as non-stick pan）Etc. people's livelihood articles for use.It is this non-to wave since early stage the 1980s
Hair property perfluoro organic compound applies rapid development industrial and civil area.The a large amount of of such product are used so that it is with each
Kind approach is entered in various surrounding mediums such as soil in global range, water body, air, is amplified by the transmission of food chain,
PFOA presence has been given in many animal tissues and human body at present.Therefore PFOA has become a kind of important global dirt
Contaminate thing, the breadth and depth of its environmental pollution exceed it is envisaged that, the research for the problem at present has become environment section
Study hotspot.
The current research of Treatment process for the perfluoroalkyl class persistent pollutant such as PFOA is very few, because of its fabulous stabilization
Property cause not degraded using conventional waste water processing method, it is also possible to cause the decomposition of its precursor to produce in processing procedure
New PFOA.Handle the alkyl compound of class containing perfluor organic wastewater, high-level oxidation technology also fast hand without plan, the hydroxyl of strong oxidizing property
Free radical is also extremely slow with the reaction rate of the perfluor class alkyl compound such as PFOA, in addition, somebody is inhaled using photochemistry, activated carbon
The methods of echoing NF membrane, treatment effect are not particularly evident.Zhao Deming etc., it have studied using ultrasonic degradation perfluor class alkane
Based compound（The dynamics of Zhao Deming etc., ultrasonic degradation PFOS and perfluoro caprylic acid, Journal of Chemical Industry and Engineering, 2011,62
（2）：829~832）, ultrasonotomography be applied to high concentration perfluor pollutant, do not reach for micro perfluor pollutant process
Ideal effect.Adsorbing separation removes organic and inorganic pollutant present in ambient water, has been considered as a kind of largely effective and normal
Processing method, removing the PFOA in water using adsorption method of separation turns into those skilled in the art's concerned issue.Using absorption
It is seldom to be separated off PFOA reports.
Shortage of resources and environmental pollution have become two big subject matters of the world today, therefore, utilize natural reproducible
Resource, development environment friendly product and technology are by as the inexorable trend of sustainable development.Luffa is that Curcurbitaceae is annual
The withered old fruit of vascular bundle in the ripening fruits of herbaceous plant sponge gourd sponge gourd in other words.Sponge gourd is that China often uses vegetable summer and autumn
There is production dish, the most provinces and regions in the whole nation, and to cultivate product, luffa is the very abundant regenerated resources of the earth, have it is light it is inexpensive,
The features such as degradable and environment-friendly, the mesh that luffa is formed by the thread fiber interweaving of multilayer, body is light, and matter is tough and tensile, it is impossible to
Fracture, while containing xylan, mannosan, galactan etc., and it has hydrophily, also with abundant dentate, very
Easily carry out chemical modification, the modified application as adsorbent in adsorption of metal ions of domestic luffa.Application No.
Luffa is disclosed in 200810034734.6 patent to exist to various metals ionic adsorption performance and luffa as adsorbent
Application in adsorption of metal ions, wherein luffa is to Cu2+And Zn2+Absorption；Natural macromolecular material is utilized as adsorbing
Agent has the advantages that renewable, degradable, environmentally friendly friendly, cheap, is important living resources.Polyacrylamide is used for being modified
Magnetic luffa has no report.
The content of the invention
An object of the present invention is to provide a kind of preparation method of polyacrylamide modified magnetic loofah adsorbent, obtains
A kind of carry out adsorbing separation of the polyacrylamide modified magnetic loofah adsorbent taken to PFOA in aqueous systems.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of polyacrylamide modified magnetic loofah adsorbent, it is characterised in that this method have with
Lower processing step：
（1）Luffa pre-processes：In the reactor, added by following composition mass percentage concentration, deionized water：50~
60%, concentrated hydrochloric acid：25 ~ 32%, stir, be cooled to room temperature, potassium permanganate：2 ~ 6%, dissolving, add luffa：10 ~ 18%, respectively
Component sum is the absolutely h of soaking at room temperature 15 ~ 20, then boils 10min, is washed with deionized after cooling to neutrality, Gu
Liquid separates, and dries, and obtains pre-processing luffa；
（2）It is prepared by magnetic luffa：In the reactor, added by following composition mass percentage concentration, deionized water：75~
82%, ferric ion：2.5 ~ 6%, ferrous ion：1.5 ~ 3%, divalent cobalt ion：0.5 ~ 2%, Aerosol OT：
0.5 ~ 1.5%, after ultrasonic dissolution, add pretreatment luffa：10 ~ 15%, each component sum is a hundred per cent, is adjusted under stirring with alkali
PH is saved between 11 ~ 13, temperature rises to 80 ± 2 DEG C of constant temperature, stirring, 10 ~ 12h of back flow reaction, and whole course of reaction is in argon gas ring
Carried out under border, after reaction terminates, be cooled to room temperature, separation of solid and liquid, wash, dry, obtain magnetic luffa；
（3）The preparation of polyacrylamide modified magnetic loofah adsorbent：In the reactor, by following composition quality percentage
Concentration adds, deionized water：72 ~ 78%, polyacrylamide：4 ~ 10%, magnetic luffa：15 ~ 20%, each component sum is percentage
Hundred, stirring reaction 5 ~ 6 days at room temperature, separation of solid and liquid, wash, dry, obtain the absorption of polyacrylamide modified magnetic luffa
Agent.
In step（1）Described in luffa for peeling stoning, clean, crush, sieving, particle diameter is between 120 ~ 160 mesh.
In step（2）Described in ferric ion be FeCl3·6H2O or FeCl3Or Fe（NO3）3Middle one or more.
In step（2）Described in ferrous ion be FeCl2·4H2O or FeCl2Or FeSO4Middle one or more.
In step（2）Described in divalent cobalt ion be CoCl2Or CoCl2·6H2O or Co（NO3）2Or Co（NO3）2·
6H2It is one or more of in O.
In step（2）Described in Fe3+∶Fe2+Mol ratio be 2.5: 1 to be optimal.
In step（2）Described in Fe2+∶Co2+Mol ratio be 2: 1 to be optimal.
In step（2）Described in alkali be one kind in sodium hydroxide or ammoniacal liquor or potassium hydroxide.
It is a further object of the present invention to provide polyacrylamide modified magnetic loofah adsorbent in aqueous systems to PFOA
Absorption, feature is：The polyacrylamide modified magnetic loofah adsorbent deionized water prepared is soaked into 2 ~ 3h, by quiet
State method is adsorbed.
The polyacrylamide modified magnetic loofah adsorbent deionized water prepared is soaked into 2 ~ 3h, inhaled by dynamic method
It is attached.
The present invention compared with the prior art, has the following advantages that and beneficial effect：
（1）The polyacrylamide modified magnetic loofah adsorbent that the present invention obtains has good physical and chemical stability
With excellent mechanical strength, adsorption capacity is big, maximum adsorption capacity up to 152.01 mg/g, it is wear-resisting can Reusability number it is reachable
More than 10 times, the speed of absorption is fast, and absorption chooses, and desorption performance is good, can be used in the range of wider soda acid.
（2）The polyacrylamide modified magnetic loofah adsorbent that the present invention obtains was both excellent with solid support material
Point, also solves the losing issue that active group polyacrylamide is applied in water environment.
（3）Stability is good, is natural green product, and regrown material, discarded object is biodegradable, its wide material sources, price
It is cheap, there is realistic meaning to pollution amelioration of ambient water etc., mitigate environmental protection pressure.
（4）The polyacrylamide modified magnetic loofah adsorbent that the present invention obtains was both excellent with solid support material
Point, PFOA are adsorbed in polyacrylamide modified magnetic loofah adsorbent, and externally-applied magnetic field can be by the absorption after the completion of absorption
Agent is separated from the water, the advantages that can be easily separated recovery.
（5）The condition for crossing range request of synthesis is easily controlled, and energy consumption is low, simple to operate, belongs to process for cleanly preparing, is easy to
Industrialized production.
Embodiment
Embodiment 1
（1）Luffa pre-processes：In the reactor, it is separately added into, deionized water：55mL, concentrated hydrochloric acid：25mL, stirring are equal
It is even, it is cooled to room temperature, potassium permanganate：3g, dissolving, adds luffa：12g, the h of soaking at room temperature 18, then 10min is boiled, after cooling
It is washed with deionized to neutrality, separation of solid and liquid, dries, obtains pre-processing luffa；
（2）It is prepared by magnetic luffa：In the reactor, it is separately added into, deionized water：82mL, FeCl3·6H2O：12g,
FeCl2·4H2O：3.5g, CoCl2·6H2O：2.0g, Aerosol OT：0.5g, after ultrasonic dissolution, add pre-
Handle luffa：14g, pH is adjusted between 11 ~ 13 with alkali under stirring, temperature rises to 80 ± 2 DEG C of constant temperature, stirring, back flow reactions
12h, whole course of reaction are carried out under ar gas environment, after reaction terminates, are cooled to room temperature, separation of solid and liquid, are washed, dry, obtain
Magnetic luffa；
（3）The preparation of polyacrylamide modified magnetic loofah adsorbent：In the reactor, it is separately added into, deionized water：
75mL, polyacrylamide：5g, magnetic luffa：20g, stirring reaction 5 days, separation of solid and liquid, are washed at room temperature, are dried, are gathered
Acrylic amide modified magnetic loofah adsorbent.
Embodiment 2
（1）Luffa pre-processes：In the reactor, it is separately added into, deionized water：100mL, concentrated hydrochloric acid：52mL, stirring are equal
It is even, it is cooled to room temperature, potassium permanganate：8g, dissolving, adds luffa：15g, the h of soaking at room temperature 17, then 10min is boiled, after cooling
It is washed with deionized to neutrality, separation of solid and liquid, dries, obtains pre-processing luffa；
（2）It is prepared by magnetic luffa：In the reactor, it is separately added into, deionized water：78mL, FeCl3：14.5g FeCl2：
4.5g, CoCl2：2.2g, Aerosol OT：1.0g, after ultrasonic dissolution, add pretreatment luffa：13g, stir
Mix it is lower with alkali adjust pH between 11 ~ 13, temperature rises to 80 ± 2 DEG C of constant temperature, stirring, back flow reaction 11h, and whole course of reaction exists
Carried out under ar gas environment, after reaction terminates, be cooled to room temperature, separation of solid and liquid, wash, dry, obtain magnetic luffa；
（3）The preparation of polyacrylamide modified magnetic loofah adsorbent：In the reactor, it is separately added into, deionized water：
78mL, polyacrylamide：4g, magnetic luffa：18g, stirring reaction 6 days, separation of solid and liquid, are washed at room temperature, are dried, are gathered
Acrylic amide modified magnetic loofah adsorbent.
Embodiment 3
（1）Luffa pre-processes：In the reactor, it is separately added into, deionized water：240mL, concentrated hydrochloric acid：84mL, stirring are equal
It is even, it is cooled to room temperature, potassium permanganate：20g, dissolving, adds luffa：40g, soaking at room temperature 16h, then 10min is boiled, after cooling
It is washed with deionized to neutrality, separation of solid and liquid, dries, obtains pre-processing luffa；
（2）It is prepared by magnetic luffa：In the reactor, it is separately added into, deionized water：150mL, Fe（NO3）3：52g,
FeSO4：13g, Co（NO3）2：7.0g, Aerosol OT：1.5g, after ultrasonic dissolution, add pretreatment luffa：
30g, pH is adjusted between 11 ~ 13 with alkali under stirring, temperature rises to 80 ± 2 DEG C of constant temperature, stirring, back flow reaction 12h, whole reaction
Process is carried out under ar gas environment, after reaction terminates, is cooled to room temperature, separation of solid and liquid, is washed, dry, obtain magnetic luffa；
（3）The preparation of polyacrylamide modified magnetic loofah adsorbent：In the reactor, it is separately added into, deionized water：
150mL, polyacrylamide：14g, magnetic luffa：34g, stirring reaction 5.5 days, separation of solid and liquid, are washed at room temperature, are dried, are obtained
To polyacrylamide modified magnetic loofah adsorbent.
Embodiment 4
（1）Luffa pre-processes：In the reactor, it is separately added into, deionized water：520mL, concentrated hydrochloric acid：240mL, stirring
Uniformly, it is cooled to room temperature, potassium permanganate：20g, dissolving, adds luffa：180g, the h of soaking at room temperature 16, then 10min is boiled, it is cold
But it is washed with deionized to neutrality, separation of solid and liquid, dries afterwards, obtains pre-processing luffa；
（2）It is prepared by magnetic luffa：In the reactor, it is separately added into, deionized water：800mL, FeCl3·6H2O：190g,
FeCl2：36g, CoCl2·6H2O：40g, Aerosol OT：6g, after ultrasonic dissolution, add pretreatment luffa：
120g, pH is adjusted between 11 ~ 13 with alkali under stirring, temperature rises to 80 ± 2 DEG C of constant temperature, stirring, back flow reaction 10.5h, entirely
Course of reaction is carried out under ar gas environment, after reaction terminates, is cooled to room temperature, separation of solid and liquid, is washed, dry, obtain magnetic sponge gourd
Network；
（3）The preparation of polyacrylamide modified magnetic loofah adsorbent：In the reactor, it is separately added into, deionized water：
750mL, polyacrylamide：100g, magnetic luffa：150g, stirring reaction 5 days, separation of solid and liquid, are washed at room temperature, are dried, are obtained
To polyacrylamide modified magnetic loofah adsorbent.
Embodiment 5
Weigh 0.10g polyacrylamide modified magnetic loofah adsorbents and be placed in 2 ~ 3h of immersion in 250mL conical flask with cover,
After filtration washing, it is in 400mg/LPFOA standard liquids, using the pH value of diluted acid or alkali regulation system as 2.0 to add 100mL concentration
In the range of ~ 11.0,4 ~ 5h of concussion absorption, takes supernatant at room temperature, with high effective liquid chromatography for measuring PFOA concentration, according to
Before and after absorption in water PFOA concentration difference, calculate the adsorption capacity of polyacrylamide modified magnetic loofah adsorbent, this hair
Absorption pH value of the bright obtained polyacrylamide modified magnetic loofah adsorbent to PFOA adsorbent in the range of 7.0 ~ 8.0
Maximum to PFOA adsorption capacity and stably, concussion absorption 4h, PFOA are adsorbed completely substantially at room temperature, PFOA absorption appearance
Amount is up to 152.01 mg/g.
Embodiment 6
Weigh 1.0g polyacrylamide modified magnetic loofah adsorbents and be placed in 2 ~ 3h of immersion in 250mL conical flask with cover,
After filtration washing, adding 100mL concentration is in 200mg/LPFOA standard liquids, using the pH value of diluted acid or alkali regulation system as
7.5, concussion absorption 4h, takes supernatant at room temperature, with high effective liquid chromatography for measuring PFOA concentration, according to water before and after absorption
Middle PFOA concentration difference, calculates clearance of the polyacrylamide modified magnetic loofah adsorbent to PFOA, and the present invention is made
The polyacrylamide modified magnetic loofah adsorbent obtained all more than 95%, reaches as high as 98% to PFOA clearance.
Claims (8)
1. a kind of preparation method of polyacrylamide modified magnetic loofah adsorbent, it is characterised in that this method has following
Processing step：
(1) luffa pre-processes：In the reactor, added by following composition mass percent, deionized water：50~60%, it is dense
Hydrochloric acid：25~32%, stir, be cooled to room temperature, potassium permanganate：2~6%, dissolving, add luffa：10~18%, respectively
Constituent mass percentage sum is absolutely 15~20h of soaking at room temperature, then boils 10min, is washed with deionized after cooling
To neutrality, separation of solid and liquid, dry, obtain pre-processing luffa；
(2) prepared by magnetic luffa：In the reactor, added by following composition mass percent, deionized water：75~82%,
Ferric ion：2.5~6%, ferrous ion：1.5~3%, divalent cobalt ion：0.5~2%, butanedioic acid di-isooctyl sulfonic acid
Sodium：0.5~1.5%, after ultrasonic dissolution, add pretreatment luffa：10~15%, each component mass percent sum is percentage
Hundred, adjust pH between 11~13 with alkali under stirring, temperature rises to 80 ± 2 DEG C of constant temperature, stirring, back flow reaction 10~12h, whole
Individual course of reaction is carried out under ar gas environment, after reaction terminates, is cooled to room temperature, separation of solid and liquid, is washed, dry, obtain magnetic silk
Melon network；
(3) preparation of polyacrylamide modified magnetic loofah adsorbent：In the reactor, add by following composition mass percent
Enter, deionized water：72~78%, polyacrylamide：4~10%, magnetic luffa：15~20%, each component mass percent
Sum is absolutely, stirring reaction 5~6 days, separation of solid and liquid, washs at room temperature, dry, obtain polyacrylamide modified magnetic
Loofah adsorbent.
2. according to a kind of preparation method of polyacrylamide modified magnetic loofah adsorbent described in claim 1, it is special
Sign is that luffa described in step (1) is peeling stoning, cleans, crushed, and sieving, particle diameter is between 120~160 mesh.
3. according to a kind of preparation method of polyacrylamide modified magnetic loofah adsorbent described in claim 1, it is special
Sign is that the ferric ion described in step (2) is FeCl3·6H2O or FeCl3Or Fe (NO3)3Middle one or more.
4. according to a kind of preparation method of polyacrylamide modified magnetic loofah adsorbent described in claim 1, it is special
Sign is that the ferrous ion described in step (2) is FeCl2·4H2O or FeCl2Or FeSO4Middle one or more.
5. according to a kind of preparation method of polyacrylamide modified magnetic loofah adsorbent described in claim 1, it is special
Sign is that the divalent cobalt ion described in step (2) is CoCl2Or CoCl2·6H2O or Co (NO3)2Or Co (NO3)2·6H2In O
It is one or more.
6. according to a kind of preparation method of polyacrylamide modified magnetic loofah adsorbent described in claim 1, it is special
Sign is that the mol ratio of ferric ion and ferrous ion is 2.5: 1 in step (2).
7. according to a kind of preparation method of polyacrylamide modified magnetic loofah adsorbent described in claim 1, it is special
Sign is that the mol ratio of step (2) ferrous ions and divalent cobalt ion is 2: 1.
8. according to a kind of preparation method of polyacrylamide modified magnetic loofah adsorbent described in claim 1, it is special
Sign is that the alkali described in step (2) is one kind in sodium hydroxide or ammoniacal liquor or potassium hydroxide.
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| CN107456954B (en) * | 2017-09-11 | 2019-02-22 | 济南大学 | A kind of preparation method of modified porous magnetic luffa complex microsphere |
| CN107511133B (en) * | 2017-09-11 | 2019-02-22 | 济南大学 | The preparation method of the modified porous magnetic luffa complex microsphere of dimercaptosuccinic acid |
| CN110280220A (en) * | 2019-06-27 | 2019-09-27 | 济南大学 | The preparation method of the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4- |
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| CN105195116A (en) * | 2015-09-21 | 2015-12-30 | 济南大学 | Preparation method of beta-cyclodextrin modified porous dextrangel adsorbent |
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| EP1193242A1 (en) * | 1998-06-02 | 2002-04-03 | Dyneon GmbH & Co. KG | Method for recovering fluorinated alkanoic acids from waste waters |
| EP2353711A1 (en) * | 2010-02-10 | 2011-08-10 | Pan-Eco S.A. | Fungal biomass preparation for the treatment of industrial wastewaters containing pollutants |
| CN102489260A (en) * | 2011-11-23 | 2012-06-13 | 清华大学 | Adsorbent for removing PFOS and PFOA in water and preparation method thereof |
| CN102500338A (en) * | 2011-11-23 | 2012-06-20 | 清华大学 | PFOA (perfluorooctanoic acid) adsorbent and preparation method thereof |
| CN104261519A (en) * | 2014-10-08 | 2015-01-07 | 深圳大学 | Method for removing perfluoro organic pollutants in waste water |
| CN105195100A (en) * | 2015-09-21 | 2015-12-30 | 济南大学 | Preparation method of beta-cyclodextrin modified loofah sponge adsorbent |
| CN105195116A (en) * | 2015-09-21 | 2015-12-30 | 济南大学 | Preparation method of beta-cyclodextrin modified porous dextrangel adsorbent |
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