CN105032311B - A kind of preparation method of one-step synthesis method porous iron oxygen microballoon - Google Patents
A kind of preparation method of one-step synthesis method porous iron oxygen microballoon Download PDFInfo
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Abstract
A kind of preparation method of one-step synthesis method porous iron oxygen microballoon, it is related to a kind of preparation method of iron microballoon.Iron oxygen micro-sphere method the invention aims to solve existing process preparation is complicated, big and high cost the problem of power consumption.Method：Aqueous sodium carbonate is added in iron chloride ethanol solution, then is stood at room temperature, then be centrifuged, remove supernatant, be precipitated material；Deposit is cleaned using distilled water, then porous iron oxygen microballoon is obtained to be dried in temperature.The size of porous iron oxygen microballoon prepared by the present invention is 5 μm~10 μm, and aperture is 1 μm~3 μm, and with magnetic, adsorbance is 70mg/g~130mg/g when adsorbing Congo red as adsorbent, is also used as toxic organic pollutant in photocatalyst treatment water body.The present invention can obtain a kind of preparation method of one-step synthesis method porous iron oxygen microballoon.
Description
Technical field
The present invention relates to a kind of preparation method of iron microballoon.
Background technology
The constituent of microballoon class material includes inorganic matter and organic matter, and its pattern is different, and size is concentrated mainly on tens
Nanometer is between hundreds of microns.The monopolizing characteristic showed according to its size, pattern and heterogeneity, can be used as micro- anti-
Answer the carrier of the catalyst such as device, adsorbent, release agent, medicine and biology enzyme, electrode material, dyestuff, microwave sorbing material, every
The materials such as heat sound insulation, can be applied to the fields such as medicine, space flight, building, industry, agricultural.Synthetic method be broadly divided into template, from
Construction from part etc..Microballoon area research is concentrated mainly on pattern, size Control and application aspect in recent years.Surface topography, composition
Composition often determines its characteristic and application field.In terms of inorganic microspheres preparation, research is concentrated mainly on containing metallization
The preparation of compound microballoon.Microballoon containing metal inorganic substance be mainly used in photoelectrocatalysis or photocatalysis, absorption, carry medicine, sensor and
The directions such as battery material.There are the magnetic properties of uniqueness due to ferriferous oxide microballoon, in recent years grinding around ferriferous oxide microballoon
Study carefully of common occurrence, but it prepares the larger iron oxygen micro-sphere method of specific surface area and mainly has hydro-thermal and solvent heat, preparation method is multiple
Miscellaneous, power consumption is big, uneconomical.Therefore, a kind of technique handy and safe is invented, raw material is cheap, is widely used, the iron of ordered porous pattern
Oxygen microballoon has very big realistic meaning.
The content of the invention
Iron oxygen micro-sphere method the invention aims to solve existing process preparation is complicated, and power consumption is big and high cost asks
Topic, and a kind of preparation method of one-step synthesis method porous iron oxygen microballoon is provided.
A kind of preparation method of one-step synthesis method porous iron oxygen microballoon, completes according to the following steps：
By concentration for 1mol/L~1.5mol/L aqueous sodium carbonate be injected into concentration for 0.006mol/L~
In the iron chloride ethanol solution of 0.009mol/L, then 20min~40min is stood at room temperature, then be in centrifugal speed
5min~15min is centrifuged under 3000r/min~5000r/min, supernatant is removed, material is precipitated；First by anhydrous second
Alcohol to deposit clean 3 times~5 times, reuse distilled water to deposit clean 3 times~5 times, then temperature be 50 DEG C~
9h~15h is dried at 70 DEG C, porous iron oxygen microballoon is obtained；
Described concentration for aqueous sodium carbonate and the concentration of 1mol/L~1.5mol/L be 0.006mol/L~
The volume ratio of the iron chloride ethanol solution of 0.009mol/L is 100 μ L:(10mL~20mL).
Principle of the invention and advantage：
First, the present invention is mainly with water and ethanol as dicyandiamide solution, with sodium carbonate and iron chloride as reaction raw materials, in room temperature
Under the conditions of the orderly porous iron oxygen microballoon of surface topography has been synthesized using a step injection method；
2nd, when certain density aqueous sodium carbonate and iron chloride ethanol solution mix, because sodium carbonate has
Characteristic that is soluble in water and being slightly soluble in ethanol, therefore can aid in forming the ethanol/water same polarity metastable state interface of moment；Carbonic acid
Sodium can promote iron chloride to be hydrolyzed at interface simultaneously, and hydrolysate is crystallized on interface, form porous iron oxygen microballoon；
3rd, the present invention is by controlling concentration, the concentration of iron chloride ethanol solution and the concentration of aqueous sodium carbonate to be
The aqueous sodium carbonate of 1mol/L~1.5mol/L is the iron chloride absolute ethyl alcohol of 0.006mol/L~0.009mol/L with concentration
In the reaction time of solution, surface topography is obtained in order and has had magnetic microballoon, its aperture is larger, and specific surface area is big, has
Magnetic, therefore can be as adsorbent and release agent treatment sewage, as photocatalyst for degrading organic pollutants in water body, as gas storage
The electrode material of material and biology sensor and battery；
4th, present invention process handy and safe, equipment is simple, can carry out at room temperature, and raw material is cheap and easy to get, with potential
Practical value；
5th, the size of porous iron oxygen microballoon prepared by the present invention is 5 μm~10 μm, and aperture is 1 μm~3 μm, with magnetic,
As adsorbent absorption it is Congo red when adsorbance be 70mg/g~130mg/g, be also used as having in photocatalyst treatment water body
Malicious organic pollution.
The present invention can obtain a kind of preparation method of one-step synthesis method porous iron oxygen microballoon.
Brief description of the drawings
Fig. 1 is the SEM figures of porous iron oxygen microballoon prepared by embodiment one.
Fig. 2 is the SEM figures of porous iron oxygen microballoon prepared by embodiment two；
Fig. 3 is that the porous iron oxygen microballoon prepared using embodiment one adsorbs Congo red front and rear digital photograph；
Fig. 4 is that the porous iron oxygen microballoon prepared using embodiment two adsorbs Congo red front and rear digital photograph.
Specific embodiment
Specific embodiment one：Present embodiment be a kind of preparation method of one-step synthesis method porous iron oxygen microballoon be by with
What lower step was completed：
By concentration for 1mol/L~1.5mol/L aqueous sodium carbonate be injected into concentration for 0.006mol/L~
In the iron chloride ethanol solution of 0.009mol/L, then 20min~40min is stood at room temperature, then be in centrifugal speed
5min~15min is centrifuged under 3000r/min~5000r/min, supernatant is removed, material is precipitated；First by anhydrous second
Alcohol to deposit clean 3 times~5 times, reuse distilled water to deposit clean 3 times~5 times, then temperature be 50 DEG C~
9h~15h is dried at 70 DEG C, porous iron oxygen microballoon is obtained；
Described concentration for aqueous sodium carbonate and the concentration of 1mol/L~1.5mol/L be 0.006mol/L~
The volume ratio of the iron chloride ethanol solution of 0.009mol/L is 100 μ L:(10mL~20mL).
The principle and advantage of present embodiment：
First, present embodiment is mainly with water and ethanol as dicyandiamide solution, with sodium carbonate and iron chloride as reaction raw materials,
The orderly porous iron oxygen microballoon of surface topography has been synthesized using a step injection method under room temperature condition；
2nd, when certain density aqueous sodium carbonate and iron chloride ethanol solution mix, because sodium carbonate has
Characteristic that is soluble in water and being slightly soluble in ethanol, therefore can aid in forming the ethanol/water same polarity metastable state interface of moment；Carbonic acid
Sodium can promote iron chloride to be hydrolyzed at interface simultaneously, and hydrolysate is crystallized on interface, form porous iron oxygen microballoon；
3rd, present embodiment is by controlling the concentration of aqueous sodium carbonate, the concentration of iron chloride ethanol solution and dense
Spend for the aqueous sodium carbonate and concentration of 1mol/L~1.5mol/L are the chlorination anhydrous ferric of 0.006mol/L~0.009mol/L
In the reaction time of ethanol solution, obtain surface topography in order and had magnetic microballoon, its aperture is larger, and specific surface area is big,
With magnetic, thus can as adsorbent and release agent treatment sewage, as photocatalyst for degrading organic pollutants in water body, as
The electrode material of gas storage material and biology sensor and battery；
4th, present embodiment technique handy and safe, equipment is simple, can carry out at room temperature, and raw material is cheap and easy to get, with latent
Practical value；
5th, the size of porous iron oxygen microballoon prepared by present embodiment is 5 μm~10 μm, and aperture is 1 μm~3 μm, is had
Magnetic, adsorbance is 70mg/g~130mg/g when adsorbing Congo red as adsorbent, is also used as photocatalyst treatment water body
Middle toxic organic pollutant.
Present embodiment can obtain a kind of preparation method of one-step synthesis method porous iron oxygen microballoon.
Specific embodiment two：Present embodiment is with the difference of specific embodiment one：It is 1.35mol/L's by concentration
Aqueous sodium carbonate is injected into the iron chloride ethanol solution that concentration is 0.0075mol/L, then is stood at room temperature
30min, then 10min is centrifuged in the case where centrifugal speed is 3500r/min, supernatant is removed, it is precipitated material；First by anhydrous
Ethanol is cleaned 3 times to deposit, reuses distilled water and deposit is cleaned 3 times, then is dried in the case where temperature is for 60 DEG C
12h, obtains porous iron oxygen microballoon.Other steps are identical with specific embodiment one.
Specific embodiment three：One of present embodiment and specific embodiment one or two difference is to be by concentration
The aqueous sodium carbonate of 1.2mol/L is injected into the iron chloride ethanol solution that concentration is 0.0085mol/L, then in room temperature
Lower standing 30min, then 10min is centrifuged in the case where centrifugal speed is 3500r/min, supernatant is removed, it is precipitated material；Make first
Deposit is cleaned with absolute ethyl alcohol 3 times, reuse distilled water and deposit is cleaned 3 times, then entered in the case where temperature is for 60 DEG C
Row dries 12h, obtains porous iron oxygen microballoon.Other steps are identical with specific embodiment one or two.
Specific embodiment four：One of present embodiment and specific embodiment one to three difference is：It is by concentration
The aqueous sodium carbonate of 1mol/L~1.2mol/L is injected into the chlorination anhydrous ferric that concentration is 0.006mol/L~0.0075mol/L
In ethanol solution, then at room temperature stand 20min~30min, then centrifugal speed be 3000r/min~3500r/min under from
Heart 5min~10min, removes supernatant, is precipitated material；Deposit is cleaned 3 times~5 times first by absolute ethyl alcohol,
Reuse distilled water to clean deposit 3 times~4 times, then 9h~12h is dried in the case where temperature is for 50 DEG C~60 DEG C, obtain
Porous iron oxygen microballoon.Other steps are identical with specific embodiment one to three.
Specific embodiment five：One of present embodiment and specific embodiment one to four difference is：It is by concentration
The aqueous sodium carbonate of 1.2mol/L~1.35mol/L is injected into the iron chloride that concentration is 0.0075mol/L~0.0085mol/L
In ethanol solution, then 30min~40min is stood at room temperature, then be 3500r/min~5000r/min in centrifugal speed
Lower centrifugation 10min~15min, removes supernatant, is precipitated material；Deposit is cleaned 3 times first by absolute ethyl alcohol
~5 times, reuse distilled water to deposit clean 4 times~5 times, then temperature be 60 DEG C~70 DEG C at be dried 12h~
15h, obtains porous iron oxygen microballoon.Other steps are identical with specific embodiment one to four.
Specific embodiment six：One of present embodiment and specific embodiment one to five difference is：It is by concentration
The aqueous sodium carbonate of 1.35mol/L~1.5mol/L is injected into the iron chloride that concentration is 0.0085mol/L~0.009mol/L
In ethanol solution, then 20min~40min is stood at room temperature, then be 3500r/min~5000r/min in centrifugal speed
Lower centrifugation 10min~15min, removes supernatant, is precipitated material；Deposit is cleaned 3 times first by absolute ethyl alcohol
~5 times, reuse distilled water to deposit clean 4 times~5 times, then temperature be 60 DEG C~70 DEG C at be dried 12h~
15h, obtains porous iron oxygen microballoon.Other steps are identical with specific embodiment one to five.
Specific embodiment seven：One of present embodiment and specific embodiment one to six difference is：Described concentration
For the aqueous sodium carbonate and the volume ratio of the iron chloride ethanol solution that concentration is 0.0075mol/L of 1.35mol/L are 100
μL:15mL.Other steps are identical with specific embodiment one to six.
Specific embodiment eight：One of present embodiment and specific embodiment one to seven difference is：Described concentration
For the aqueous sodium carbonate and the volume ratio of the iron chloride ethanol solution that concentration is 0.0085mol/L of 1.2mol/L are 100 μ
L:15mL.Other steps are identical with specific embodiment one to seven.
Specific embodiment nine：One of present embodiment and specific embodiment one to eight difference is：Described concentration
For the aqueous sodium carbonate and concentration of 1mol/L~1.35mol/L are the chlorination anhydrous ferric of 0.006mol/L~0.0075mol/L
The volume ratio of ethanol solution is 100 μ L:15mL.Other steps are identical with specific embodiment one to eight.
Specific embodiment ten：One of present embodiment and specific embodiment one to nine difference is：Described concentration
For the aqueous sodium carbonate and concentration of 1mol/L~1.2mol/L are the chlorination anhydrous ferric second of 0.006mol/L~0.0085mol/L
The volume ratio of alcoholic solution is 100 μ L:15mL.Other steps are identical with specific embodiment one to nine.
Beneficial effects of the present invention are verified using following examples：
Embodiment one：A kind of preparation method of one-step synthesis method porous iron oxygen microballoon is completed according to the following steps：
By concentration for the aqueous sodium carbonate of 1.35mol/L is injected into the chlorination anhydrous ferric second that concentration is 0.0075mol/L
In alcoholic solution, then 30min is stood at room temperature, then 10min is centrifuged in the case where centrifugal speed is 3500r/min, remove supernatant, obtain
To deposit；Deposit is cleaned 3 times first by absolute ethyl alcohol, is reused distilled water and deposit is cleaned 3 times, then
12h is dried at being 60 DEG C in temperature, porous iron oxygen microballoon is obtained；
Described concentration is the chlorination anhydrous ferric second of 0.0075mol/L for the aqueous sodium carbonate and concentration of 1.35mol/L
The volume ratio of alcoholic solution is 100 μ L:15mL.
Fig. 1 is the SEM figures of porous iron oxygen microballoon prepared by embodiment one；The size of porous microsphere is mainly divided as can be seen from Figure 1
Cloth is at 5 μm~10 μm, and the hole on single microballoon is uniform in size, quite similar with morning glory, and the pore size of different balls is different, but
The aperture of porous iron oxygen ball is mainly distributed on 1 μm~3 μm.The sodium carbonates' presence that it is critical only that of porous microsphere, carbon can be formed
Sour sodium has characteristic that is soluble in water and being slightly soluble in ethanol, can aid in forming an ethanol/water same polarity metastable in injection instant
State interface；Sodium carbonate can promote iron chloride to be hydrolyzed at interface simultaneously, and hydrolysate occurs caused by crystallization on interface.
The size of porous iron oxygen microballoon prepared by embodiment one is 5 μm~10 μm, and aperture is 1 μm~3 μm, with magnetic,
Adsorbance is 70mg/g~130mg/g when adsorbing Congo red as adsorbent；It is also used as having in photocatalyst treatment water body
Malicious organic pollution.
As the application test of adsorbent：
It is the porous iron oxygen microballoon for adding 15mg embodiments one to prepare in the Congo red aqueous solution of 100mg/L to 15mL concentration
Porous iron oxygen ball after, sustained oscillation 2h under darkroom.Treatment effect is shown in that Fig. 3, Fig. 3 are the porous iron oxygen prepared using embodiment one
Digital photograph before and after microballoon absorption is Congo red；By the Congo red aqueous solution after the porous iron oxygen ball absorption that embodiment one is obtained
Color fade.
Embodiment two：A kind of preparation method of one-step synthesis method porous iron oxygen microballoon is completed according to the following steps：
By concentration for the aqueous sodium carbonate of 1.2mol/L is injected into the iron chloride absolute ethyl alcohol that concentration is 0.0085mol/L
In solution, then 30min is stood at room temperature, then 10min is centrifuged in the case where centrifugal speed is 3500r/min, remove supernatant, obtain
Deposit；Deposit is cleaned 3 times first by absolute ethyl alcohol, is reused distilled water and deposit is cleaned 3 times, then
Temperature obtains porous iron oxygen microballoon to be dried 12h at 60 DEG C；
Described concentration is the iron chloride absolute ethyl alcohol of 0.0085mol/L for the aqueous sodium carbonate and concentration of 1.2mol/L
The volume ratio of solution is 100 μ L:15mL.
Fig. 2 is the SEM figures of porous iron oxygen microballoon prepared by embodiment two；The size of porous microsphere is mainly divided as can be seen from Figure 2
Cloth is at 5 μm~10 μm, and the hole on single microballoon is uniform in size, quite similar with morning glory, and the pore size of different balls is different, but
The aperture of porous iron oxygen ball is mainly distributed on 1 μm~3 μm.The sodium carbonates' presence that it is critical only that of porous microsphere, carbon can be formed
Sour sodium has characteristic that is soluble in water and being slightly soluble in ethanol, can aid in forming an ethanol/water same polarity metastable in injection instant
State interface；Sodium carbonate can promote iron chloride to be hydrolyzed at interface simultaneously, and hydrolysate occurs caused by crystallization on interface.
The size of porous iron oxygen microballoon prepared by embodiment two is 5 μm~10 μm, and aperture is 1 μm~3 μm, with magnetic,
As adsorbent absorption it is Congo red when adsorbance be 70mg/g~130mg/g, be also used as having in photocatalyst treatment water body
Malicious organic pollution.
As the application test of adsorbent：
It is the porous iron oxygen ball for adding 15mg embodiments two to prepare in the Congo red aqueous solution of 100mg/L to 15mL concentration
Afterwards, sustained oscillation 2h under darkroom, treatment effect is shown in that Fig. 4, Fig. 4 are that the porous iron oxygen microballoon prepared using embodiment two adsorbs the Congo
Digital photograph before and after red；By the color fade of the Congo red aqueous solution after the porous iron oxygen ball absorption that embodiment two is obtained.
Claims (10)
1. a kind of preparation method of one-step synthesis method porous iron oxygen microballoon, it is characterised in that a kind of one-step synthesis method porous iron oxygen is micro-
The preparation method of ball is completed according to the following steps：
By concentration for the aqueous sodium carbonate of 1mol/L~1.5mol/L is injected into concentration for 0.006mol/L~0.009mol/L
Iron chloride ethanol solution in, then at room temperature stand 20min~40min, then centrifugal speed be 3000r/min~
5min~15min is centrifuged under 5000r/min, supernatant is removed, material is precipitated；First by absolute ethyl alcohol to deposit
Cleaning 3 times~5 times, reuses distilled water and deposit is cleaned 3 times~5 times, then is done in the case where temperature is for 50 DEG C~70 DEG C
Dry 9h~15h, obtains porous iron oxygen microballoon；
Described concentration is 0.006mol/L~0.009mol/L for the aqueous sodium carbonate and concentration of 1mol/L~1.5mol/L
Iron chloride ethanol solution volume ratio be 100 μ L:(10mL~20mL).
2. the preparation method of a kind of one-step synthesis method porous iron oxygen microballoon according to claim 1, it is characterised in that will be dense
Spend for the aqueous sodium carbonate of 1.35mol/L is injected into the iron chloride ethanol solution that concentration is 0.0075mol/L, then
30min is stood at room temperature, then 10min is centrifuged in the case where centrifugal speed is 3500r/min, remove supernatant, be precipitated material；It is first
Deposit is cleaned 3 times using absolute ethyl alcohol first, distilled water is reused and deposit is cleaned 3 times, then be 60 DEG C in temperature
Under be dried 12h, obtain porous iron oxygen microballoon.
3. the preparation method of a kind of one-step synthesis method porous iron oxygen microballoon according to claim 1, it is characterised in that will be dense
Spend for the aqueous sodium carbonate of 1.2mol/L is injected into the iron chloride ethanol solution that concentration is 0.0085mol/L, then
30min is stood at room temperature, then 10min is centrifuged in the case where centrifugal speed is 3500r/min, remove supernatant, be precipitated material；It is first
Deposit is cleaned 3 times using absolute ethyl alcohol first, distilled water is reused and deposit is cleaned 3 times, then be 60 DEG C in temperature
Under be dried 12h, obtain porous iron oxygen microballoon.
4. the preparation method of a kind of one-step synthesis method porous iron oxygen microballoon according to claim 1, it is characterised in that will be dense
Spend for the aqueous sodium carbonate of 1mol/L~1.2mol/L is injected into the iron chloride that concentration is 0.006mol/L~0.0075mol/L
In ethanol solution, then 20min~30min is stood at room temperature, then be 3000r/min~3500r/min in centrifugal speed
Lower centrifugation 5min~10min, removes supernatant, is precipitated material；First by absolute ethyl alcohol to deposit clean 3 times~
5 times, reuse distilled water and deposit cleaned 3 times~4 times, then 9h~12h is dried in the case where temperature is for 50 DEG C~60 DEG C,
Obtain porous iron oxygen microballoon.
5. the preparation method of a kind of one-step synthesis method porous iron oxygen microballoon according to claim 1, it is characterised in that will be dense
Spend for the aqueous sodium carbonate of 1.2mol/L~1.35mol/L is injected into the chlorine that concentration is 0.0075mol/L~0.0085mol/L
In change anhydrous ferric ethanol solution, then 30min~40min is stood at room temperature, then be 3500r/min~5000r/ in centrifugal speed
10min~15min is centrifuged under min, supernatant is removed, material is precipitated；First by absolute ethyl alcohol to deposit cleaning 3
It is secondary~5 times, reuse distilled water and deposit is cleaned 4 times~5 times, then 12h is dried in the case where temperature is for 60 DEG C~70 DEG C
~15h, obtains porous iron oxygen microballoon.
6. the preparation method of a kind of one-step synthesis method porous iron oxygen microballoon according to claim 1, it is characterised in that will be dense
Spend for the aqueous sodium carbonate of 1.35mol/L~1.5mol/L is injected into the chlorine that concentration is 0.0085mol/L~0.009mol/L
In change anhydrous ferric ethanol solution, then 20min~40min is stood at room temperature, then be 3500r/min~5000r/ in centrifugal speed
10min~15min is centrifuged under min, supernatant is removed, material is precipitated；First by absolute ethyl alcohol to deposit cleaning 3
It is secondary~5 times, reuse distilled water and deposit is cleaned 4 times~5 times, then 12h is dried in the case where temperature is for 60 DEG C~70 DEG C
~15h, obtains porous iron oxygen microballoon.
7. a kind of preparation method of one-step synthesis method porous iron oxygen microballoon according to claim 1, it is characterised in that concentration
For the aqueous sodium carbonate and the volume ratio of the iron chloride ethanol solution that concentration is 0.0075mol/L of 1.35mol/L are 100
μL:15mL。
8. a kind of preparation method of one-step synthesis method porous iron oxygen microballoon according to claim 1, it is characterised in that concentration
For the aqueous sodium carbonate and the volume ratio of the iron chloride ethanol solution that concentration is 0.0085mol/L of 1.2mol/L are 100 μ
L:15mL。
9. a kind of preparation method of one-step synthesis method porous iron oxygen microballoon according to claim 1, it is characterised in that concentration
For the aqueous sodium carbonate and concentration of 1mol/L~1.35mol/L are the chlorination anhydrous ferric of 0.006mol/L~0.0075mol/L
The volume ratio of ethanol solution is 100 μ L:15mL.
10. a kind of preparation method of one-step synthesis method porous iron oxygen microballoon according to claim 1, it is characterised in that concentration
For the aqueous sodium carbonate and concentration of 1mol/L~1.2mol/L are the chlorination anhydrous ferric second of 0.006mol/L~0.0085mol/L
The volume ratio of alcoholic solution is 100 μ L:15mL.
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