CN106215860A - A kind of by sonochemistry method synthesis fluorine ion absorber ZrO2al2o3the method of/GO - Google Patents
A kind of by sonochemistry method synthesis fluorine ion absorber ZrO2al2o3the method of/GO Download PDFInfo
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- CN106215860A CN106215860A CN201610632383.3A CN201610632383A CN106215860A CN 106215860 A CN106215860 A CN 106215860A CN 201610632383 A CN201610632383 A CN 201610632383A CN 106215860 A CN106215860 A CN 106215860A
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- 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
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0211—Compounds of Ti, Zr, Hf
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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
- B01J20/02—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
- B01J20/08—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 comprising aluminium oxide or hydroxide; comprising bauxite
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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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
Abstract
The open one of the present invention synthesizes fluorine ion absorber ZrO by sonochemistry method2‑Al2O3The method of/GO, the method is by ZrOCl2 .8H2O、F127、AlCl3.6H2O、MgSO4Dissolve and form colourless transparent solution in ethanol, after adding graphene oxide, after sonic oscillation generation phonochemical reaction, and separating, washing and drying and processing, the ZrO obtained2‑Al2O3The thick product of/GO refluxes in apparatus,Soxhlet's, product separating, washing again and drying and processing, obtains fluorine ion absorber ZrO2‑Al2O3/GO.The present invention response time is short, simple to operate, and efficiently, power consumption is few, low cost, gained ZrO2‑Al2O3/ GO product has higher Adsorption effect to fluorion, can be used for the improvement of fluoride pollution waste water on a large scale.
Description
Technical field
The present invention relates to a kind of by sonochemistry method synthesis fluorine ion absorber ZrO2-Al2O3The method of/GO, particularly belongs to
Sonochemistry technical field.
Background technology
Ultrasonication is found in nineteen twenty-seven the earliest to the impact of compound, since then, sonic oscillation effect just by with
In Organic substance and the synthesis of inorganic matter, it is referred to as sonochemistry synthetic method.Comparatively speaking, ultrasound wave is more safer than microwave, because
Its frequency is lower.Nowadays, ultrasound wave is as effective energy source, it is possible to changes the chemical property of substrate thus accelerates chemistry instead
The effect answered is widely known.When ul-trasonic irradiation is in aqueous media, owing to sound wave is to the lasting expansion of solution and compression
Circulation, produces positive/negative-pressure persistently alternately in the solution.This behavior results in a series of minute bubbles, and these are stingy
Bubble is filled with vaporized steam.These minute bubbles are sound wave accumulation of energy in radiative process, therefore these minute bubbles meetings
Expansion reaches a critical point, before they cave in rapidly, it may appear that of short duration hole.When caving in, each minute bubbles are
One heat generating spot, can produce the highest temperature (5500 DEG C) and pressure (thousand of atmospheric pressure), can interrupt chemical bond, produces
Free radical, thus cause a series of phonochemical reaction.Sonochemistry synthetic method have the time short, power consumption less, efficiency high,
Receive significant attention.
Fluorion is a kind of serious pollutant, and organism can be caused serious harm by the fluorine of excess.The most in the world
There is Fluorine of Drinking Water excessive problem in a lot of places, administers Fluorine of Drinking Water and pollute the focus having become current environment pollution control
Problem.Absorption method is because of its low cost, and simple to operate becoming applies to obtain one of most commonly used fluoride pollution Treatment process.Absorption at present
The preparation method of agent mainly has the sedimentation method, hydro-thermal method, calcination method etc., often also exists that response time length, power consumption be big, complex operation
Etc. problem.In order to solve this series of problems, the preparation method developing new adsorbent is imperative.
Under this technical background, we have developed a kind of by sonochemistry method synthesis fluorine ion absorber ZrO2-Al2O3/GO
Method.Only ultrasound wave need to be utilized raw material effect 5min, so that it may to promote to bring it about chemical reaction and generate product.The letter of described method
Singly, efficient, power consumption is few, and products obtained therefrom has efficient Adsorption performance to fluorion.
Summary of the invention
It is an object of the invention to provide a kind of by sonochemistry method synthesis fluorine ion absorber ZrO2-Al2O3The side of/GO
Method, the method comprises the steps:
(1) by ZrOCl2 .8H2O, F127(polyoxyethylene/polyoxypropylene/polyoxyethylene amphiphilic block copolymer),
AlCl3.6H2O、MgSO4Dissolve and form colourless transparent solution in ethanol；Described ZrOCl2 .8H2O and AlCl3.6H2O mole
Ratio is 1:2 to 1:0.5.
(2) in the solution of step (1) gained, graphene oxide is added, after ultrasound wave generation phonochemical reaction, then
Mechanical agitation 15min；Described graphene oxide and stepZrOCl2 .8H2The mass ratio of O is 1:2.4.
(3) in step (2) products therefrom, add deionized water and the mixed liquor of ethanol that volume ratio is 1:5, continue to stir
Carrying out sucking filtration separation after mixing 1h, gained filter cake ethanol, deionized water replace each washing 3 times, are then dried overnight in 50 DEG C, i.e.
Obtain ZrO2-Al2O3The thick product of/GO.
(4) ZrO2-Al2O3The thick product of/GO in apparatus,Soxhlet's with the ethanol that volume ratio is 150:2.3 and concentrated hydrochloric acid
Mixed liquor separate at 95 DEG C of reflux 48h, followed by sucking filtration, gained filter cake ethanol, deionized water replace each washing 3 times,
It is dried overnight at 50 DEG C again, obtains ZrO2-Al2O3/GO。
In step (2), the ultrasonic power that described phonochemical reaction uses is 250W, and the ultrasonication time is 5min.
Advantages of the present invention: the response time is short, simple to operate, efficiently, power consumption is few, and low cost, products obtained therefrom is to fluorion
There is higher Adsorption effect, can be used for the improvement of fluoride pollution waste water on a large scale.
Accompanying drawing explanation
Fig. 1 is fluorine ion absorber ZrO obtained by the embodiment of the present invention 12-Al2O3/ the GO adsorption isotherm to fluorion
Figure.
Detailed description of the invention
Hereinafter embodiments of the invention are described in further detail, but the present embodiment is not limited to the present invention.
Embodiment 1
Graphene oxide (GO) is prepared with the method for the regular oxidation graphite of report.
By 0.48g ZrOCl2 .8H2O、0.1 g F127、0.72g AlCl3.6H2O、0.36g MgSO4It is dissolved in 100 ml second
Alcohol forms clear solution (ZrOCl2 .8H2O and AlCl3.6H2The mol ratio of O is 1:2).Add 0.2 g GO afterwards, with 250W's
Power ultrasonic action-reaction 5 min, then mechanical agitation 15 min.Then the volume of 100 ml deionized waters and ethanol it is slowly added into
Than the mixed solution for 1:5, after continuing stirring 1 h, sucking filtration separation solid.Gained solid is the most each with ethanol, deionized water
Wash 3 times, then 50 DEG C drying over night, obtain ZrO2-Al2O3The thick product of/GO.
By the ZrO of gained2-Al2O3Mixed at 150 ml ethanol and 2.30 ml concentrated hydrochloric acid of/GO thick product apparatus,Soxhlet's
With in solution, 95 DEG C backflow 48 h.Reacted rear taking-up ethanol, deionized water replaces each washing 3 times, then 50 DEG C are dried one
In evening, obtain final product.It is 57.4mg/g to the maximal absorptive capacity of fluorion.
Embodiment 2
Graphene oxide (GO) is prepared with the method for the regular oxidation graphite of report.
By 0.48g ZrOCl2 .8H2O、0.1 g F127、0.36g AlCl3.6H2O、0.36g MgSO4It is dissolved in 100 ml second
Alcohol forms clear solution (ZrOCl2 .8H2O and AlCl3.6H2The mol ratio of O is 1:1).Add 0.2 g GO afterwards, with 250W's
Power ultrasonic action-reaction 5 min, then mechanical agitation 15 min.Then the volume of 100 ml deionized waters and ethanol it is slowly added into
Than the mixed solution for 1:5, after continuing stirring 1 h, sucking filtration separation solid.Gained solid is the most each with ethanol, deionized water
Wash 3 times, then 50 DEG C drying over night, obtain ZrO2-Al2O3The thick product of/GO.
By the ZrO of gained2-Al2O3Mixed at 150 ml ethanol and 2.30 ml concentrated hydrochloric acid of/GO thick product apparatus,Soxhlet's
With in solution, 95 DEG C backflow 48 h.Reacted rear taking-up ethanol, deionized water replaces each washing 3 times, then 50 DEG C are dried one
In evening, obtain final product.It is 57.3mg/g to the maximal absorptive capacity of fluorion.
Embodiment 3
Graphene oxide (GO) is prepared with the method for the regular oxidation graphite of report.
By 0.48g ZrOCl2 .8H2O、0.1 g F127、0.18g AlCl3.6H2O、0.36g MgSO4It is dissolved in 100 ml second
Alcohol forms clear solution (ZrOCl2 .8H2O and AlCl3.6H2The mol ratio of O is 1:0.5).Add 0.2 g GO afterwards, with 250W
Power ultrasonic action-reaction 5 min, then mechanical agitation 15 min.Then the body of 100 ml deionized waters and ethanol it is slowly added into
The long-pending ratio mixed solution for 1:5, after continuing stirring 1 h, sucking filtration separation solid.By gained solid with ethanol, deionized water alternately
Each washing 3 times, then 50 DEG C drying over night, obtain ZrO2-Al2O3The thick product of/GO.
By the ZrO of gained2-Al2O3Mixed at 150 ml ethanol and 2.30 ml concentrated hydrochloric acid of/GO thick product apparatus,Soxhlet's
With in solution, 95 DEG C backflow 48 h.Reacted rear taking-up ethanol, deionized water replaces each washing 3 times, then 50 DEG C are dried one
In evening, obtain final product.It is 102mg/g to the maximal absorptive capacity of fluorion.
Claims (2)
1. one kind synthesizes fluorine ion absorber ZrO by sonochemistry method2-Al2O3The method of/GO, it is characterised in that: described side
Method comprises the steps:
(1) by ZrOCl2 .8H2O、F127、AlCl3.6H2O、MgSO4Dissolve and form colourless transparent solution in ethanol；Described
ZrOCl2 .8H2O and AlCl3.6H2The mol ratio of O is 1:2 to 1:0.5；
(2) in the solution of step (1) gained, graphene oxide is added, after ultrasound wave generation phonochemical reaction, then machinery
Stirring 15min；Described graphene oxide and stepZrOCl2 .8H2The mass ratio of O is 1:2.4；
(3) in step (2) products therefrom, add deionized water and the mixed liquor of ethanol that volume ratio is 1:5, continue stirring 1h
After carry out sucking filtration separation, gained filter cake ethanol, deionized water replace each washing 3 times, are then dried overnight in 50 DEG C, to obtain final product
ZrO2-Al2O3The thick product of/GO；
(4) ZrO2-Al2O3The thick product of/GO in apparatus,Soxhlet's with the ethanol that volume ratio is 150:2.3 and the mixing of concentrated hydrochloric acid
Liquid separates at 95 DEG C of reflux 48h, followed by sucking filtration, and gained filter cake ethanol, deionized water replace each washing 3 times, then 50
It is dried overnight at DEG C, obtains ZrO2-Al2O3/GO。
One the most according to claim 1 synthesizes fluorine ion absorber ZrO by sonochemistry method2-Al2O3The method of/GO,
It is characterized in that: in step (2), the ultrasonic power that described phonochemical reaction uses is 250W, and the ultrasonication time is
5min。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107413294A (en) * | 2017-05-19 | 2017-12-01 | 西安石油大学 | A kind of method that graphene-supported silver handles high Oil repellent domestic water |
| CN110614076A (en) * | 2019-10-14 | 2019-12-27 | 西安工程大学 | Preparation method of zirconium dioxide/aluminum oxide composite adsorption material |
| CN111644150A (en) * | 2020-06-11 | 2020-09-11 | 南昌航空大学 | Preparation method of phosphate adsorbent based on 3D rGO/zirconium dioxide composite material |
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| JPS61220787A (en) * | 1985-03-25 | 1986-10-01 | Miyoshi Oil & Fat Co Ltd | Treatment of water |
| CN103861559A (en) * | 2014-03-12 | 2014-06-18 | 陕西科技大学 | Zirconia-modified graphene and method for removing fluorine ions in water |
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2016
- 2016-08-05 CN CN201610632383.3A patent/CN106215860B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61220787A (en) * | 1985-03-25 | 1986-10-01 | Miyoshi Oil & Fat Co Ltd | Treatment of water |
| CN103861559A (en) * | 2014-03-12 | 2014-06-18 | 陕西科技大学 | Zirconia-modified graphene and method for removing fluorine ions in water |
Non-Patent Citations (2)
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| JIUYA ZHU等: "Fluoride removal from aqueous solution by Al(III)–Zr(IV) binary oxide adsorbent", 《APPLIED SURFACE SCIENCE》 * |
| SARAT KANRAR等: "Preparation, characterization and evaluation of fluoride adsorption efficiency from water of iron-aluminium oxide-graphene oxide composite material", 《CHEMICAL ENGINEERING JOURNAL》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107413294A (en) * | 2017-05-19 | 2017-12-01 | 西安石油大学 | A kind of method that graphene-supported silver handles high Oil repellent domestic water |
| CN110614076A (en) * | 2019-10-14 | 2019-12-27 | 西安工程大学 | Preparation method of zirconium dioxide/aluminum oxide composite adsorption material |
| CN111644150A (en) * | 2020-06-11 | 2020-09-11 | 南昌航空大学 | Preparation method of phosphate adsorbent based on 3D rGO/zirconium dioxide composite material |
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