CN106000337B - A kind of preparation method of magnetism catalytic adsorption material - Google Patents
A kind of preparation method of magnetism catalytic adsorption material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 25
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 19
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 230000005389 magnetism Effects 0.000 title claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 14
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000001116 FEMA 4028 Substances 0.000 claims abstract description 9
- 229960004853 betadex Drugs 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 239000012263 liquid product Substances 0.000 claims description 12
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 7
- 239000002202 Polyethylene glycol Substances 0.000 claims description 7
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims 1
- 229910002804 graphite Inorganic materials 0.000 claims 1
- 239000010439 graphite Substances 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 229910021389 graphene Inorganic materials 0.000 abstract description 7
- 150000001875 compounds Chemical class 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 3
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 abstract description 2
- 230000001588 bifunctional effect Effects 0.000 abstract description 2
- 239000006249 magnetic particle Substances 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 230000008929 regeneration Effects 0.000 abstract description 2
- 238000011069 regeneration method Methods 0.000 abstract description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 abstract 1
- 235000011175 beta-cyclodextrine Nutrition 0.000 abstract 1
- 239000012265 solid product Substances 0.000 description 8
- 238000002955 isolation Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000007792 addition Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- 229920001353 Dextrin Polymers 0.000 description 2
- 239000004375 Dextrin Substances 0.000 description 2
- 235000019425 dextrin Nutrition 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000010215 titanium dioxide Nutrition 0.000 description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000002122 magnetic nanoparticle Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/069—Hybrid organic-inorganic polymers, e.g. silica derivatized with organic groups
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
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- B01J35/33—
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- B01J35/39—
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
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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
- 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
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
Abstract
The invention belongs to field of new material preparation, specifically using solvent-thermal method, using ethylene glycol as solvent, by ethylenediamine beta cyclodextrin/graphene supermolecule (EDA CD GO), with TiO2（P25）, nano magnetic particle Fe3O4The compound method for preparing magnetic catalytic adsorption material.The nano ferriferrous oxide of this method generation can be with the compound obtained bifunctional material with catalytic adsorption of P25, EDA CD GO.The material has higher yield, can solve current material regeneration and recycle the problems such as difficult, realize the effect of efficient, environmentally protective.These all make the present invention have extremely wide application prospect.
Description
Technical field
The invention belongs to field of new material preparation, specifically disclose a kind of preparation side of magnetic catalytic adsorption material
Method.
Background technology
At present, environmental pollution has become one of the problem of most being paid close attention to for the mankind.Exist in the environment such as water body, air and soil stone
Many organic pollutions for destroying the ecological balance, these organic pollution stones only can voluntarily be degraded by biology on a small quantity, most of
It is difficult to it is degraded.Relative to the method for common processing organic pollution：Physical, biodegradation technique and chemical method etc., light is urged
Changing degradation has many advantages, such as efficient, environmentally friendly, easy to operate and becomes one of most promising method.Light-catalyzed reaction is come
It says, TiO2（P25 titanium dioxides）It is a kind of semiconductor of most study, this is because its cheap, disposable, large specific surface area
And the advantages that stablizing.
Ethylenediamine-beta-cyclodextrin/graphene supermolecule（EDA-CD-GO）Hybrid is a kind of supermolecule material of nanoscale
Material, the identification of cyclodextrin section and a series of substrate of inclusion, and the complexing of the proton of C=C of graphene oxide and functional group, such as-
COOH is with-OH meetings and with functional group-NH2Strong hydrogen bond is generated with the organic pollution of-OH；With nano magnetic particle Fe3O4
It is compound to prepare nano-magnetic compound, the high-ratio surface energy of magnetic nano-particle is on the one hand reduced, avoids it caused by reunion
Particle diameter distribution unevenness and poor biocompatibility the defects of；On the other hand its surface can be made from the direct invasion of external environment,
Maintain its chemical stability and magnetic property.By TiO2Photocatalytic degradation and the Magneto separate of low energy consumption, the EDA-CD-GO of small particle
It is effectively compound, Magnetic Isolation can be carried out, realizes that catalytic adsorption is difunctional, for solving the organic pollution ring of current getting worse
Border is protected, and realizes the reasonable using with important theory and realistic meaning of resource.
Invention content
The purpose of the present invention：In order to solve the problems, such as that current organic pollutant only can voluntarily be degraded by biology on a small quantity,
The present invention provides a kind of methods that catalytic adsorption material is prepared by EDA-CD-GO.
Technical scheme is as follows：It is a kind of magnetism catalytic adsorption material preparation method, the preparation method include with
Lower step：（1）By graphene oxide powder（GO）It adds in deionized water, after 1 ~ 4h of ultrasound, adds in KOH and ethylenediamine-β-ring
Dextrin（EDA-CD）, 10 ~ 50min is stirred at room temperature, it is ensured that is thoroughly mixed, at 70 DEG C ~ 90 DEG C, is reacted 20 ~ 30h, obtain
Even dark solution, centrifuges solid-liquid product, and washing solid-liquid product to pH value is 7（It is adjusted by acid-base solution）, vacuum does
Ethylenediamine-beta-cyclodextrin/graphene supermolecule (EDA-CD-GO) is prepared in dry solid-liquid product, spare；Technological process such as Fig. 1
It is shown；（2）Again using ethylene glycol as solvent, using solvent-thermal method, by step（1）The EDA-CD-GO supermolecules and TiO prepared2
And FeCl3·6H2O is uniformly mixed, and after stirring 1 ~ 3h, adds NaAc（CH3COONa）And polyethylene glycol, it is mixed again
0.5~1h；It fills this blend into autoclave, is heated to 170 ~ 200 DEG C, react 12 ~ 18h, using magnetism, detach solid-liquid
A kind of catalytic adsorption material, i.e. EDA-CD-GO/ TiO is prepared in product, drying solid-liquid product2 /Fe3O4, technological process is such as
Shown in Fig. 2.
Wherein, the mass ratio of EDA-CD and GO is 1:0.05 ~ 0.4, the mass ratio with KOH is 1:0.1 ~ 0.6,
EDA-CD-GO and FeCl3•6H2The mass ratio of O is 1:5 ~ 10, the mass ratio with solvent ethylene glycol is 1:10 ~ 20, with NaAc
Mass ratio be 1:20 ~ 50, the mass ratio with polyethylene glycol is 1:5 ~ 20, with TiO2Mass ratio be 1:0.5~2.
Used graphene oxide powder is one kind in technical grade；Used ethylenediamine-beta-cyclodextrin is β-ring
One kind in dextrin derivative；Used TiO2For Degussa P25, the EDA-CD-GO is beta-cyclodextrin derivative and stone
One kind in supermolecule prepared by black alkene.
Advantageous effect：Compared with prior art, the present invention has the following advantages：The nanometer four generated in reaction process aoxidizes
Three-iron can be with P25（TiO2）, EDA-CD-GO it is compound be made with catalytic adsorption bifunctional material.The material has higher
Yield can solve current material regeneration and recycle the problems such as difficult, realize the effect of efficient, environmentally protective.These all make this hair
It is bright that there is extremely wide application prospect.
Description of the drawings
Fig. 1 EDA-CD-GO preparation technology flow charts of the present invention；Fig. 2 is the process flow chart of catalytic adsorption material of the present invention；
Fig. 3 and Fig. 4 is respectively EDA-CD-GO and nano ferriferrous oxide, P25 combination products EDA-CD-GO/ in the embodiment of the present invention 1
P25 /Fe3O4Transmission electron microscope figure and powder x-ray diffraction spectrogram.
Specific embodiment
Embodiment 1, a kind of preparation method of magnetic catalytic adsorption material, its step are as follows：（1）0.15g GO additions are gone
In ionized water, after ultrasonic 1.5h, 0.2g KOH and 1g ethylenediamine-beta-cyclodextrins are added in（EDA-CD）, 30min is stirred at room temperature,
Ensure to be thoroughly mixed, at 80 DEG C, reaction for 24 hours, obtains uniform dark solution, centrifuges solid-liquid product, washing solid production
Object to pH value is 7, and ethylenediamine-beta-cyclodextrin/graphene supermolecule (EDA-CD-GO) is prepared in vacuum drying solid product,
It is spare；（2）After the ethylene glycol of 0.1g EDA-CD-GO and 50mL are sufficiently mixed, 0.1gP25 is added in, adds 0.5g
FeCl3•6H2O is stirred 2 hours, sequentially adds 3.6g NaAc and 1.0g polyethylene glycol, is stirred 1 hour；It fills this blend into
In reaction kettle, at 180 DEG C, 16h is reacted, liquid consolidates product Magnetic Isolation, transmission electron microscope figure such as Fig. 3 institutes of solid product
Show, it is seen that the distribution of particles of EDA-CD-GO and P25 is less uniform；X-ray diffraction spectrogram as shown in figure 4, visible 2 θ be 18.2 °,
Peak at 30.0 °, 35.5 °, 43.2 °, 53.2 °, 57.1 ° and 62.9 ° is respectively belonging to Fe3O4Nano-particle（111）,
（220）,（311）,（400）,（422）,（511）And（440）Crystal face, 2 θ show point in the characteristic peak that 25 ° are titanium dioxide P25
It is magnetic catalytic adsorption material from the solid product after solid-liquid product（EDA-CD-GO/P25 /Fe3O4）.
Embodiment 2, a kind of preparation method of magnetic catalytic adsorption material, its step are as follows：（1）0.1g GO additions are gone
In ionized water, after ultrasonic 1h, 0.25g KOH and 1g ethylenediamine-beta-cyclodextrins are added in（EDA-CD）, 20min is stirred at room temperature, really
Guarantor is thoroughly mixed, and at 85 DEG C, reacts 22h, obtains uniform dark solution, centrifuge solid-liquid product, washs solid product
It is 7 to pH value, ethylenediamine-beta-cyclodextrin/graphene supermolecule (EDA-CD-GO) is prepared in vacuum drying solid product, standby
With；（2）After the ethylene glycol of 0.1g EDA-CD-GO and 50mL are sufficiently mixed, 0.15gP25 is added in, adds 0.5g
FeCl3•6H2O is stirred 2 hours, sequentially adds 3.6g NaAc and 1.0g polyethylene glycol, is stirred 1 hour；It fills this blend into
In reaction kettle, at 180 DEG C, 16h is reacted, liquid consolidates product Magnetic Isolation, and solid product is magnetic catalytic adsorption material.
Embodiment 3, a kind of preparation method of magnetic catalytic adsorption material, its step are as follows：（1）0.15g GO additions are gone
In ionized water, ultrasound adds in 0.2g KOH and 1g ethylenediamine-beta-cyclodextrins after 2 hours（EDA-CD）, 40min is stirred at room temperature,
Ensure to be thoroughly mixed, at 85 DEG C, react 22h, obtain uniform dark solution, centrifuge solid-liquid product, washing solid production
Object to pH value is 7, and ethylenediamine-beta-cyclodextrin/graphene supermolecule (EDA-CD-GO) is prepared in vacuum drying solid product,
It is spare；（2）After the ethylene glycol of 0.1g EDA-CD-GO and 50mL are sufficiently mixed, 0.2gP25 is added in, adds 0.5g
FeCl3•6H2O is stirred 2 hours, sequentially adds 3.3g NaAc and 1.0g polyethylene glycol, is stirred 1 hour；It fills this blend into
In reaction kettle, at 200 DEG C, 16h is reacted, liquid consolidates product Magnetic Isolation, and solid product is magnetic catalytic adsorption material.
Claims (1)
1. a kind of preparation method of magnetism catalytic adsorption material, it is characterised in that：The preparation method includes the following steps：
（1）Graphene oxide powder GO is added in deionized water, after 0.5 ~ 4h of ultrasound, adds in KOH and ethylenediamine-beta-cyclodextrin
EDA-CD at room temperature, stirs 10 ~ 50min；At 70 DEG C ~ 90 DEG C, 20 ~ 30h is reacted, obtains uniform dark solution, centrifugation point
From solid-liquid product, washing solid-liquid product to pH value is 7, and ethylenediamine-beta-cyclodextrin/graphite is prepared in vacuum drying solid-liquid product
Alkene supermolecule EDA-CD-GO, it is spare；
（2）Again using ethylene glycol as solvent, using solvent-thermal method, by step（1）The EDA-CD-GO supermolecules and TiO prepared2With
FeCl3·6H2O is uniformly mixed, and after stirring 1 ~ 3h, adds NaAc and polyethylene glycol, and 0.5 ~ 2h is mixed again；It will mixing
Object is fitted into autoclave, is heated to 170 ~ 200 DEG C, and reaction 12 ~ for 24 hours, magnetism is utilized, detaches solid-liquid product, drying solid-liquid
A kind of catalytic adsorption material, i.e. EDA-CD-GO/ TiO is prepared in product2 /Fe3O4；Wherein, the mass ratio of EDA-CD and GO
It is 1:0.05 ~ 0.4, the mass ratio with KOH is 1:0.1 ~ 0.6, EDA-CD-GO and FeCl3•6H2The mass ratio of O is 1: 5
~ 10, the mass ratio with solvent ethylene glycol is 1:10 ~ 20, the mass ratio with NaAc is 1:20 ~ 50, the matter with polyethylene glycol
Amount is than being 1:5 ~ 20, with TiO2Mass ratio be 1:0.5~2.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102716730A (en) * | 2012-07-11 | 2012-10-10 | 济南大学 | Preparation method for novel nano magnetic cyclodextrin/graphene biological adsorption material |
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