CN106492761A - A kind of preparation method of magnetic hydrogel microsphere - Google Patents

A kind of preparation method of magnetic hydrogel microsphere Download PDF

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Publication number
CN106492761A
CN106492761A CN201610933831.3A CN201610933831A CN106492761A CN 106492761 A CN106492761 A CN 106492761A CN 201610933831 A CN201610933831 A CN 201610933831A CN 106492761 A CN106492761 A CN 106492761A
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preparation
microsphere
soluble polymer
water soluble
hydrogel microsphere
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魏宏亮
刘静静
楚晖娟
何娟
朱靖
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Henan University of Technology
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Henan University of Technology
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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
    • B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • 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
    • 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
    • B01J20/28014—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 form
    • B01J20/28047—Gels
    • 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
    • C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
    • 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 a kind of preparation method of magnetic hydrogel microsphere, belongs to sewage treatment area.The method first passes through coprecipitation to be prepared and is loaded with Fe3O4The graphene oxide of magnetic nano-particle（GO@Fe3O4）, then by the GO@Fe3O4With water soluble polymer（Such as sodium carboxymethyl cellulose CMC）Mixed merga pass spray drying method prepares the magnetic composite aquogel microsphere of tool（Such as CMC/GO@Fe3O4）.Prepared composite aquogel microsphere has good swelling behavior and larger specific surface area, greatly improve the adsorption efficiency to pollutant, improve absorbed species and adsorbance of the hydrogel to pollutant, and be easily isolated, can be used as the adsorbent of organic dyestuff and heavy metal ion in industrial wastewater.

Description

A kind of preparation method of magnetic hydrogel microsphere
Technical field
The present invention relates to sewage treatment area, more particularly to a kind of magnetic graphene-based composite aquogel microsphere of tool Preparation method.
Background technology
Containing substantial amounts of pollutant such as heavy metal ion and organic dyestuff etc. in industrial wastewater, its processing mode is in recent years The study hotspot for coming.For the processing mode such as traditional electro-deposition and filtration, physical absorption has low cost, operation letter Singly, the advantages of not causing secondary pollution.Even so, traditional adsorbing material includes activated carbon, wood flour, cinder, volcanic ash etc. Generally existing adsorption efficiency is low, Selective adsorption is poor, difficult recovery the shortcomings of.It is huge that loose structure inside hydrogel gives which Specific surface area, can provide substantial amounts of attachment site for pollutant absorption.Therefore, a kind of good pollutant adsorption material is considered Material is subject to the parent of numerous research worker to rely.
However, the aquogel system that is studied at present such as chitin hydrogel is general to the adsorbance and the rate of adsorption of pollutant All over relatively low, such as document Water Res., 2004,38,2643-2650; J. Mater. Chem. A, 2013, 1, 1992-2001; Carbon, 2011, 49, 827-837.The reason for adsorbance is low is mainly polymeric matrix and pollutant sheet Body interaction is weaker, and the low volume larger mainly due to hydrogel of the rate of adsorption and limited percent opening are unfavorable for pollutant Diffusion wherein.For adsorbance, inorganic nano-particle is generally incorporated into aquogel system, Jin Erzeng by low problem people Strong composite aquogel and the interaction of pollutant.However, but failing to solve well for the low problem of the rate of adsorption.This Outward, also there is low preparation efficiency, high cost, be difficult to large-scale production in above-mentioned hydrogel.
Content of the invention
For the problems referred to above, it is an object of the invention to provide a kind of process is simple, the rate of adsorption is high, microsphere is easily isolated simultaneously The preparation method of the magnetic hydrogel microsphere of the suitable industrialized production of reusable edible, so as to get hydrogel microsphere to a huge sum of money Category particle（Such as hexavalent chromium Cr6+）There is excellent absorption property with organic dyestuff.
For reaching the object of the invention, adopt the following technical scheme that：
The preparation method of described magnetic hydrogel microsphere comprises the steps：
（1）Graphite oxide is scattered in deionized water, ultrasound is peeled off, and obtains the dispersion liquid of graphene oxide.Then in inertia Fe is added under atmosphere2+Iron salt and Fe3+Iron salt and alkaline matter, obtain graphene oxide after reaction（GO）And nanometer Fe3O4Mixed Compound GO@Fe3O4.
（2）Water soluble polymer is dissolved in distilled water, cross-linking agent and GO@Fe is then added wherein3O4, ultrasound point It is stirred for after dissipating.Finally, mixed solution is passed through spray dryer and prepares the magnetic hydrogel microsphere of tool.
The step（1）Middle graphite oxide both can be prepared by Hummer methods, it is also possible to by Staudenmaier methods Prepare.
Inert atmosphere can be that one or two in nitrogen and argon are mixed by any ratio and form.
Fe2+Iron salt selects FeSO4、FeCl2·4H2O、Fe(NO3)2In one or more, Fe3+Iron salt selects Fe2(SO4)3、 FeCl3·6H2O、Fe(NO3)2In one or more.Alkaline matter can be NH3·H2O、NaOH、Ca(OH)2In one kind Or it is several.
The step（1）The concentration of the dispersion liquid of middle graphene oxide is 1-10 mg/mL, Fe in source of iron2+And Fe3+Rub You are than being 2：1-1：3, alkaline matter addition accounts for the 1-10 wt.% of total solution weight.
The step（2）In water soluble polymer can be cellulose derivative such as methylcellulose, ethyl cellulose One or more of element, hydroxyethyl cellulose, carboxymethyl cellulose, hydroxypropyl methyl cellulose etc., cross-linking agent are citric acid, second One or more in dialdehyde, glutaraldehyde, divinylsulfone, multi-anhydride, epoxychloropropane.
The step（2）In water soluble polymer solid content be 1-2%；The addition of cross-linking agent is water solublity high score The 1-10 wt.% of sub- weight；GO@Fe3O4Addition account for the 1-20 wt.% of water soluble polymer weight.It is preferred that：GO@Fe3O4 Addition account for the 8-10 wt.% of water soluble polymer weight.
The step（2）It is 110～160 °C that the parameter of middle spray-drying installation is set to inlet temperature, and sample size is 500-800 mL/h, air mass flow are 60～90%.
Compared with prior art, of the invention by graphene oxide（GO）With nano ferriferrous oxide Fe3O4Particle is simultaneously introduced The hydrogel microsphere of magnetic is prepared in water miscible natural polymer subsystem and by spray drying method.Such material and side Method has advantages below：（1）GO and nanometer Fe3O4Absorbed species and adsorbance of the hydrogel to pollutant can be improved；（2） Fe3O4Nanoparticle gives microsphere certain magnetic, makes it easy to separate；（3）The structure design of microsphere imparts such hydrogel Larger specific surface area, greatly improves the adsorption efficiency to pollutant；（4）Gained GO@Fe3O4Yield high, be 80-95%. And spray drying method prepares complex microsphere and there is process is simple, low cost, easy large-scale production.The method has good Market application foreground.
Description of the drawings
Fig. 1 is the scanning electron microscope of the magnetic hydrogel microsphere prepared by the embodiment of the present invention 1（SEM）Figure.
Fig. 2 be the embodiment of the present invention 1 prepared by hydrogel microsphere under different pH, Cr6+Adsorbance change rectangular histogram.
Specific embodiment
For the present invention is better described, technical scheme is readily appreciated, the present invention's is typical but non-limiting Embodiment is as follows：
Embodiment 1：
（1）By the graphite oxide ultrasonic disperse prepared by the Hummers methods of 0.5 g in 100 mL deionized waters, concentration is obtained GO dispersion liquids for 5 mg/mL.Then, under nitrogen atmosphere, add the iron salt of 1.5 g wherein（Fe2+And Fe3+Mol ratio For 1:2）With 0.2g NaOH solutions, 30 min are reacted, GO@Fe are obtained3O4Mixture, dried for standby after centrifugation.
（2）Take 5 g CMC to be dissolved under 60 °C in 500 mL distilled water, then add the GO@of 0.435 g wherein Fe3O4With the citric acid of 0.2 g, 3 h of magnetic agitation after ultrasonic disperse, then with spray dryer prepare GO@Fe3O4Content is 8 The CMC complex microspheres of wt%, are labeled as CMC/GO@Fe3O4.The parameter of the spray-drying installation is set to inlet temperature for 150 ～160 °C, sample size is 600-800 mL/h, and air mass flow is 80～90%.Finally, by obtained complex microsphere at 90 ° Seal after 5 h are dried in the baking oven of C standby.
Additionally, pure CMC microspheres（It is labeled as CMC）CMC microspheres only containing GO（It is labeled as CMC/GO）Also identical method is used Prepare and be used as comparative example.
Obtained in of the invention, the sem analysis result of complex microsphere shows：CMC/GO@Fe3O4The particle diameter of complex microsphere is 2-5 μm（Fig. 1）, microsphere has good controllability and monodispersity.With Cr6+For pollutant model, the absorption property of microsphere is tested （Cr6+Initial concentration be 200 mg/L, 15 °C of test temperature）, Fig. 2 as shown by data：（1）At pH=4, CMC based aquagels The adsorbance of microsphere is close to maximum；（2）The presence of GO significantly enhances composite aquogel microsphere to Cr6+Adsorbance, and receive Rice Fe3O4The introducing of particle not only increases the adsorbance of its heavy metal ion, while the magnetic of complex microsphere has also speeded up again The rate of departure of microsphere is closed, is easy to which to recycle.For example, 8 wt% GO@Fe3O4The CMC complex microspheres of content are to Cr6+Full Reached 35 mg/g with adsorbance, compared with comparative example in CMC and the adsorbance of CMC/GO increase significantly and the complex microsphere Adsorption equilibrium can be reached in 30 min.The special construction of complex microsphere has been effectively ensured its quick adsorption to pollutant.And And be easily isolated, beneficial to recycling.
Embodiment 2：
The present embodiment 2 prepares CMC/GO@Fe by 1 identical mode of embodiment3O4Composite aquogel microsphere, differs only in this reality Apply the GO@Fe of the complex microsphere in example3O4Content be 2 wt%.As a result show, the hydrogel microsphere in the present embodiment pH= It is 9 mg/g to the adsorbance of hexavalent chromium when 4.
Embodiment 3：
The present embodiment 3 prepares CMC/GO@Fe by 1 identical mode of embodiment3O4Composite aquogel microsphere, differs only in this reality Apply the GO@Fe of the complex microsphere in example3O4Content be 4 wt%.As a result show, the hydrogel microsphere in the present embodiment pH= It is 17 mg/g to the adsorbance of hexavalent chromium when 4.
Embodiment 4：
The present embodiment 4 prepares CMC/GO@Fe by 1 identical mode of embodiment3O4Composite aquogel microsphere, differs only in this reality Apply the GO@Fe of the complex microsphere in example3O4Content be 6 wt%.As a result show, the hydrogel microsphere in the present embodiment pH= It is 24 mg/g to the adsorbance of hexavalent chromium when 4.
Embodiment 5：
（1）By the graphite oxide ultrasonic disperse prepared by the Staudenmaier methods of 1 g in 100 mL deionized waters, obtain dense Spend the GO dispersion liquids for 10 mg/mL.Then, under nitrogen atmosphere, add the iron salt of 1.5 g wherein（Fe2+And Fe3+Rub You are than being 1:1）With 0.1 g NH3·H2O solution, reacts 30 min, obtains GO@Fe3O4Mixture, after centrifugation dry Stand-by.
（2）Take 5 g methylcellulose to be dissolved in 500 mL distilled water, then add the GO@Fe of 1 g wherein3O4With 1 g Glutaraldehyde, 3 h of magnetic agitation after ultrasonic disperse, then GO@Fe are prepared with spray dryer3O4It is micro- that content is that the CMC of 10 wt% is combined Ball, is labeled as CMC/GO@Fe3O4.It is 120～130 °C that the parameter of the spray-drying installation is set to inlet temperature, sample size For 500-600 mL/h, air mass flow is 70～80%.Finally, obtained complex microsphere is dried in 90 °C of baking oven 5 Seal after h standby.As a result show, the hydrogel microsphere in the present embodiment is 47 at pH=4 to the adsorbance of hexavalent chromium mg/g.
Prepared complex microsphere can be used as a class broad spectrum type adsorbent in terms of water process, with green, efficient, easy point From the features such as, good market application foreground.

Claims (6)

1. a kind of preparation method of magnetic hydrogel microsphere, is characterized in that：Comprise the steps：
（1）Graphite oxide is scattered in deionized water, ultrasound is peeled off, and obtains the dispersion liquid of graphene oxide；Then in inertia Fe is added under atmosphere2+Iron salt and Fe3+Iron salt and alkaline matter, obtain graphene oxide after reaction（GO）And nanometer Fe3O4Mixed Compound GO@Fe3O4；
（2）Water soluble polymer is dissolved in distilled water, cross-linking agent and GO@Fe is then added wherein3O4, after ultrasonic disperse It is stirred for；Finally, mixed solution is passed through spray dryer and prepares magnetic hydrogel microsphere；
Step（1）Described alkaline matter selects NH3·H2O、NaOH、Ca(OH)2In one or more；
Step（2）Described water soluble polymer selects methylcellulose, ethyl cellulose, hydroxyethyl cellulose, carboxymethyl cellulose One or more in element, hydroxypropyl methyl cellulose；Cross-linking agent selects citric acid, Biformyl, glutaraldehyde, divinylsulfone, many One or more in first anhydride, epoxychloropropane.
2. the preparation method of magnetic hydrogel microsphere according to claim 1, is characterized in that：Step（1）Described Fe2+Ferrum Salt selects FeSO4、FeCl2·4H2O、Fe(NO3)2In one or more；Fe3+Iron salt selects Fe2(SO4)3、FeCl3·6H2O、Fe (NO3)2In one or more.
3. the preparation method of magnetic hydrogel microsphere according to claim 1, is characterized in that：The step（1）Middle oxidation The dispersion liquid concentration of Graphene is 1-10 mg/mL； Fe2+And Fe3+Mol ratio be 2：1-1：3；Alkaline matter addition accounts for molten The 1-10 wt.% of liquid gross weight.
4. the preparation method of magnetic hydrogel microsphere according to claim 1, is characterized in that：The step（2）In
The solid content of water soluble polymer is 1-2%；1-10 wt.% of the addition of cross-linking agent for water soluble polymer weight； GO@Fe3O4Addition for water soluble polymer weight 1-20 wt.%.
5. the preparation method of magnetic hydrogel microsphere according to claim 4, is characterized in that：GO@Fe3O4Addition be The 8-10 wt.% of water soluble polymer weight.
6., according to the preparation method of one of them described magnetic hydrogel microsphere of claim 1-5, it is characterized in that：The step （2）The parameter of middle spray-drying installation is set to inlet temperature for 110～160 °C, and sample size is 500-800 mL/h, air Flow is 60～90%.
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CN107746841A (en) * 2017-09-07 2018-03-02 天津大学 A kind of amphion magnetic coupling aquogel fixed enzyme carrier and preparation method
CN107964396A (en) * 2017-11-30 2018-04-27 陕西理工大学 A kind of graphene photothermal conversion materiat preparation method
CN108393071A (en) * 2018-03-21 2018-08-14 广东电网有限责任公司电力科学研究院 A kind of compound adsorbent and preparation method thereof
CN108554412A (en) * 2018-05-11 2018-09-21 江西理工大学 A kind of preparation method and applications of large scale high porosity Fe doping photocatalyzing magnetic porous microsphere
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CN110721664B (en) * 2019-10-10 2021-12-17 浙江海洋大学 Preparation method of mussel shell powder/carboxymethyl cellulose composite gel adsorbent
CN110918129A (en) * 2019-11-25 2020-03-27 华南理工大学 Cellulose/graphene oxide/ferroferric oxide composite hydrogel catalytic carrier applied to sewage treatment field and preparation method thereof
CN110776159A (en) * 2019-12-05 2020-02-11 江苏苏讯新材料科技有限公司 Chromium-plated steel plate wastewater recycling system
CN111841512A (en) * 2020-07-16 2020-10-30 兰州大学 Material capable of enriching and separating thorium and preparation method thereof
CN114197201A (en) * 2022-01-11 2022-03-18 四川大学 Magnetic graphene oxide modified carbon fiber and preparation method and application thereof
CN115382547A (en) * 2022-09-09 2022-11-25 四川农业大学 Iron-carbon microsphere composite catalyst for Fenton-like system, preparation method and application
CN115382547B (en) * 2022-09-09 2024-03-15 四川农业大学 Iron-carbon microsphere composite catalyst for Fenton-like system, and preparation method and application thereof

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Application publication date: 20170315