CN109019622A - A method of preparing clay loaded nano magnetite - Google Patents
A method of preparing clay loaded nano magnetite Download PDFInfo
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- CN109019622A CN109019622A CN201810903144.6A CN201810903144A CN109019622A CN 109019622 A CN109019622 A CN 109019622A CN 201810903144 A CN201810903144 A CN 201810903144A CN 109019622 A CN109019622 A CN 109019622A
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- clay
- loaded nano
- nano magnetite
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- microwave
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Compounds Of Iron (AREA)
Abstract
A method of clay loaded nano magnetite is prepared, first disperses clay in the ethylene glycol solution dissolved with trivalent iron salt and divalent iron salt；Thereafter a certain amount of sodium acetate ethylene glycol solution is mixed with and is transferred in round-bottomed flask, be placed in microwave chemical reactor the cooling for reflux under certain microwave power and react；After reacting cooling, by sample centrifugation, wash, it is dry in vacuum oven, obtain product, the nano magnetite of the clay mineral load of this method preparation has the characteristics that good dispersion, prepares quick, reproducible, while preparation process simplicity, economical and energy saving, can be mass-produced.
Description
Technical field
The present invention relates to nanocomposite preparation technical fields, in particular to a kind of to prepare clay loaded nano magnetite
Method.
Background technique
Magnetic iron ore be it is a kind of information storage, material, medicine and environmental area extensive application material.In environment dirt
It contaminates object and administers aspect, since its magnetism can simply be divided after it is applied to environment by Magnetic Isolation means
From, avoid the material after processing pollutant from generating secondary pollution to surrounding medium, meanwhile, reproducibility is contained in the structure of matter
Fe (II), to Cr (VI), the high-valence states heavy metal such as Tc (VII), U (VI) and Hg (II) has a stronger reducing power, and by
To extensive concern and research.The partial size of nano magnetite has important influence to the removal ability of pollutant, and partial size is smaller right
The removal efficiency of pollutant is higher, however, nano particle is smaller, free energy is bigger, easier aggregation.The nano particle of formation
Aggregation will limit nano material significantly to the effect of pollutant process.It is received by the porous material loading of bigger serface
Rice magnetic iron ore can effectively balance activity, capacity, reusing and the bio-compatibility of nano magnetite.
Clay mineral refers to some hydrosilicate mineral containing based on aluminium, magnesium etc., they are composition clay rock and soil
Essential mineral.In addition to sepiolite, palygorskite tool chain layer structure, remaining has a layer structure.Clay mineral is according to its unit
Crystal layer construction feature can be divided into: 1:1 type clay, 2:1 type clay, 2:2 type clay mineral and layer chain structure clay pit
Object.Clay mineral have the characteristics that price it is low, there are extensive and high specific surface area, be reported and can be used as magnetic nanoparticle
Support materials.However, that there are processes is complicated, takes a long time, imitates for the preparation method of existing clay mineral load nano magnetite
The problems such as rate is not high.
Summary of the invention
In order to overcome the disadvantages of the above prior art, clay loaded nano magnetic is prepared the purpose of the present invention is to provide a kind of
The method of iron ore, can efficiently, easily prepare clay mineral load nano magnetite, have simple process, it is environmental-friendly, can
Repeated strong, the characteristics of can be mass-produced.
In order to achieve the above object, the technical scheme adopted by the invention is as follows:
A method of clay loaded nano magnetite being prepared, steps are as follows:
Step 1: by clay abrasive and crossing 200 meshes, be dried for standby after deionized water cleaning；
Step 2: by FeCl3·6H2O (Iron(III) chloride hexahydrate) and soluble divalent iron salt are dissolved in ethylene glycol, wherein three
Valence iron and soluble ferrous molar ratio are (1.5-2.5): 1, step 1 gained clay is dispersed in acquired solution, is stirred
Uniformly；
Step 3: anhydrous sodium acetate (CH will be dissolved with3COONa ethylene glycol (EG) solution) is added to step 2 acquired solution
In, CH in solution3COONa and ferric molar ratio are (3-5): 1, clay quality is the 5%-20% of solution quality, sufficiently
Mix to obtain mixed solution；
Step 4: step 3 gained mixed solution is placed in microwave chemical reactor the cooling for reflux under certain microwave power
Certain time is reacted, after reacting cooling, by sample centrifugation, ethanol wash, drying, obtains product.
Clay mineral content in the clay is higher than 80%.
The divalent iron salt is one of frerrous chloride or ferrous sulfate.
Ferric iron and soluble ferrous molar ratio are 2:1 in the mixed solution.
CH in step 3 solution3COONa and ferric molar ratio are 4:1.
The microwave chemical reactor microwave frequency is 2.45GHZ.
The microwave power is 50%-100%.
The microwave reaction time is 20-60 minutes.
The step 4 is dried using vacuum oven.
The present invention having the beneficial effect that compared with prior art
The present invention prepares clay mineral load nano magnetite using microwave reaction, and microwave reaction method is a kind of green, high
Synthetic method is imitated, generated time is short, magnetic iron ore good dispersion in the composite material of synthesis.It is multiple with clay-magnetic iron ore of existing report
Condensation material preparation method is compared, and the pH and reaction temperature of finely regulating system are not needed in preparation process, reacts easy to operate, can
It is repeated strong.
Specific embodiment
The present invention is described in further details below with reference to embodiment.
Embodiment 1
Step 1: kaolin being ground, 200 mesh sieve is crossed, is dried for standby after deionized water cleaning.
Step 2: taking the clay of 100g step 1, be added to 0.4L dissolved with 5.4gFeCl3·6H2O and 2.0g FeCl2·
4H2In the ethylene glycol solution of O, stir 30 minutes.
Step 3: 6.4g CH will be dissolved with3The 100mL EG solution of COONa is added in step 2 acquired solution, sufficiently mixed
Conjunction obtains mixed solution.
Step 4: mixed solution being transferred in the round-bottomed flask of 1L, is placed in microwave chemical reactor in 80% microwave function
Cooling for reflux reacts 30min under rate, and the microwave frequency is 2.45GHZ.After reacting cooling, sample centrifugation, alcohol are washed
It washs, after dry in vacuum oven, obtains the nano magnetite composite material of kaolinite load.
Embodiment 2
Step 1: bentonite being ground, 200 mesh sieve is crossed, is dried for standby after deionized water cleaning.
Step 2: taking the clay of 100g step 1, be added to 0.5L dissolved with 10.8gFeCl3·6H2O and 5.5g FeSO4·
7H2In the ethylene glycol solution of O, stir 30 minutes.
Step 3: 12.8g CH will be dissolved with3The 100mL ethylene glycol solution of COONa is added in step 2 acquired solution, is filled
Divide and is mixed to get mixed solution.
Step 4: mixed solution being transferred in the round-bottomed flask of 1L, is placed in microwave chemical reactor in 80% microwave function
Cooling for reflux reacts 60min under rate, and the microwave frequency is 2.45GHZ.After reacting cooling, sample centrifugation, alcohol are washed
It washs, after dry in vacuum oven, obtains the nano magnetite composite material of alta-mud load.
Embodiment 3
Step 1: vermiculite being ground, 200 mesh sieve is crossed, is dried for standby after deionized water cleaning.
Step 2: taking the clay of 100g step 1, be added to 0.9L dissolved with 21.6gFeCl3·6H2O and 8.0g FeCl2·
4H2In the ethylene glycol solution of O, stir 30 minutes.
Step 3: 25.6g CH will be dissolved with3The 100mL ethylene glycol solution of COONa is added in step 2 acquired solution, is filled
Divide and is mixed to get mixed solution.
Step 4: mixed solution being transferred in the round-bottomed flask of 2L, is placed in microwave chemical reactor in 100% microwave
Cooling for reflux reacts 30min under power, and the microwave frequency is 2.45GHZ.After reacting cooling, by sample centrifugation, alcohol
It washs, after dry in vacuum oven, obtains the nano magnetite composite material of vermiculite load.
Embodiment 4
Step 1: attapulgite being ground, 200 mesh sieve is crossed, is dried for standby after deionized water cleaning.
Step 2: taking the clay of 100g step 1, be added to 0.9L dissolved with 21.6gFeCl3·6H2O and 8.0g FeCl2·
4H2In the ethylene glycol solution of O, stir 30 minutes.
Step 3: 25.6g CH will be dissolved with3The 100mL EG solution of COONa is added in step 2 acquired solution, sufficiently
It is mixed to get mixed solution.
Step 4: mixed solution being placed in microwave chemical reactor, cooling for reflux reacts under 80% microwave power
30min, the microwave frequency are 2.45GHZ.After reacting cooling, sample is centrifuged, ethanol wash, is done in vacuum oven
After dry, the nano magnetite composite material of attapulgite loaded is obtained.
Embodiment 5
Step 1: sepiolite being ground, 200 mesh sieve is crossed, is dried for standby after deionized water cleaning.
Step 2: taking the clay of 100g step 1, be added to 0.9L dissolved with 16.2gFeCl3·6H2O and 6.0g FeCl2·
4H2In the ethylene glycol solution of O, stir 30 minutes.
Step 3: 19.2g CH will be dissolved with3The 100mL EG solution of COONa is added in step 2 acquired solution, sufficiently
It is mixed to get mixed solution.
Step 4: mixed solution being placed in microwave chemical reactor, cooling for reflux reacts under 50% microwave power
60min, the microwave frequency are 2.45GHZ.After reacting cooling, sample is centrifuged, ethanol wash, is done in vacuum oven
After dry, sepiolite supported nano magnetite composite material is obtained.
Embodiment 6
Step 1: galapectite being ground, 200 mesh sieve is crossed, is dried for standby after deionized water cleaning.
Step 2: taking the clay of 100g step 1, be added to 0.9L dissolved with 21.6gFeCl3·6H2O and 11.2g
FeSO4·7H2In the ethylene glycol solution of O, stir 30 minutes.
Step 3: 25.6g CH will be dissolved with3The 100mL EG solution of COONa is added in step 2 acquired solution, sufficiently
It is mixed to get mixed solution.
Step 4: mixed solution being placed in microwave chemical reactor, cooling for reflux reacts under 80% microwave power
60min.After reacting cooling, sample is centrifuged, ethanol wash, it is dry in vacuum oven, obtain receiving for galapectite load
Rice magnetic iron ore composite material.
Claims (9)
1. a kind of method for preparing clay loaded nano magnetite, which comprises the steps of:
Step 1: by clay abrasive and crossing 200 meshes, be dried for standby after deionized water cleaning；
Step 2: by FeCl3·6H2O (Iron(III) chloride hexahydrate) and soluble divalent iron salt are dissolved in ethylene glycol, wherein ferric iron
It is (1.5-2.5) with soluble ferrous molar ratio: 1, step 1 gained clay is dispersed in acquired solution, is stirred evenly；
Step 3: anhydrous sodium acetate (CH will be dissolved with3COONa ethylene glycol (EG) solution) is added in step 2 acquired solution, molten
CH in liquid3COONa and ferric molar ratio are (3-5): 1, clay quality is the 5%-20% of solution quality, is sufficiently mixed
Mixed solution；
Step 4: step 3 gained mixed solution being placed in microwave chemical reactor the cooling for reflux under certain microwave power and is reacted
Certain time, by sample centrifugation, ethanol wash, drying, obtains product after reacting cooling.
2. a kind of method for preparing clay loaded nano magnetite according to claim 1, which is characterized in that the clay
In clay mineral content be higher than 80%.
3. a kind of method for preparing clay loaded nano magnetite according to claim 1, which is characterized in that the divalent
Molysite is one of frerrous chloride or ferrous sulfate.
4. a kind of method for preparing clay loaded nano magnetite according to claim 1, which is characterized in that the mixing
Ferric iron and soluble ferrous molar ratio are 2:1 in solution.
5. a kind of method for preparing clay loaded nano magnetite according to claim 1, which is characterized in that the step
CH in 3 solution3COONa and ferric molar ratio are 4:1.
6. a kind of method for preparing clay loaded nano magnetite according to claim 1, which is characterized in that the microwave
Chemical reactor microwave frequency is 2.45GHZ.
7. a kind of method for preparing clay loaded nano magnetite according to claim 1, which is characterized in that the microwave
Power is 50%-100%.
8. a kind of method for preparing clay loaded nano magnetite according to claim 1, which is characterized in that the microwave
Reaction time is 20-60 minutes.
9. a kind of method for preparing clay loaded nano magnetite according to claim 1, which is characterized in that the step
4 are dried using vacuum oven.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110075789A (en) * | 2019-05-23 | 2019-08-02 | 陕西科技大学 | A kind of cyanobacteria magnetic based on the modified preparation of attapulgite catches the preparation method of agent |
| CN110075788A (en) * | 2019-05-23 | 2019-08-02 | 陕西科技大学 | A kind of cyanobacteria magnetic based on the modified preparation of sepiolite catches the preparation method of agent |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948135A (en) * | 2016-05-03 | 2016-09-21 | 上海交通大学 | Monodisperse porous magnetic submicrosphere and preparation method thereof |
-
2018
- 2018-08-09 CN CN201810903144.6A patent/CN109019622A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948135A (en) * | 2016-05-03 | 2016-09-21 | 上海交通大学 | Monodisperse porous magnetic submicrosphere and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 于生慧: "纳米环境矿物材料的制备及重金属处理研究", 《中国博士学位论文全文数据库工程科技I辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110075789A (en) * | 2019-05-23 | 2019-08-02 | 陕西科技大学 | A kind of cyanobacteria magnetic based on the modified preparation of attapulgite catches the preparation method of agent |
| CN110075788A (en) * | 2019-05-23 | 2019-08-02 | 陕西科技大学 | A kind of cyanobacteria magnetic based on the modified preparation of sepiolite catches the preparation method of agent |
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Application publication date: 20181218 |