CN108607514A - A kind of preparation method of aminated magnetic porous microspheres - Google Patents
A kind of preparation method of aminated magnetic porous microspheres Download PDFInfo
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- CN108607514A CN108607514A CN201810496740.7A CN201810496740A CN108607514A CN 108607514 A CN108607514 A CN 108607514A CN 201810496740 A CN201810496740 A CN 201810496740A CN 108607514 A CN108607514 A CN 108607514A
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- porous microspheres
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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
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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
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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
- B01J20/28—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
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
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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
- B01J20/28—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
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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
- B01J20/28—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
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention discloses a kind of preparation method of aminated magnetic porous microspheres, step includes：By FeCl3·6H2O, anhydrous sodium acetate and 1,6 hexamethylene diamines are dissolved in ethylene glycol and form clear solution；Step 1 gained clear solution is sealed in autoclave, is heated under the conditions of 196 200 DEG C and aminated magnetic porous microspheres is obtained by the reaction；It is saved backup after drying.Nano-scale magnetic iron oxide particle with stronger heavy metal adsorption can fast and effeciently be prepared by preparation method of the present invention, and prepared nano-scale magnetic iron oxide particle be easy to store it is spare.
Description
Technical field
The invention belongs to environment water treatment field more particularly to a kind of aminated magnetic porous microspheres for water process
Preparation method.
Background technology
With the fast development of global industry, various toxic heavy metals are with industries such as leather, papermaking, weaving, printing and dyeing
Waste water be discharged into environment water, serious threat is caused to health.Therefore, effective heavy metal in water is developed to go
Except technology is of great significance to public health and sustainable economic development.
Invention content
Goal of the invention：A kind of aminated magnetic porous microspheres preparation side that can effectively remove heavy metal in water is provided
Method.
Technical solution：A kind of preparation method of aminated magnetic porous microspheres of the present invention, includes the following steps：
Step 1, by FeCl3·6H2O, anhydrous sodium acetate and 1,6- hexamethylene diamines be dissolved in ethylene glycol formed it is transparent molten
Liquid；
Step 2, step 1 gained clear solution is sealed in autoclave, reaction is heated under the conditions of 196-200 DEG C
Obtain aminated magnetic porous microspheres；
Step 3, it is saved backup after drying.
Further, in step 1, used FeCl3·6H2O, anhydrous sodium acetate, 1,6- hexamethylene diamines and ethylene glycol
Amount ratio is 1g：5.6g：3.6g：30mL.
Further, it in step 1, is stirred simultaneously with the speed of agitator of 980-1020rpm in dissolving.Using the stirring
Rotating speed can realize the Quick uniform dissolving of material.
Further, in step 2, the heating reaction time in stainless steel autoclave is 4.5-5.5 hours.
Further, in step 2, used autoclave is the stainless steel reaction under high pressure of teflon lined
Kettle.
Further, in step 2, reaction is heated under the conditions of 198 DEG C.
Further, it in step 2, after aminated magnetic porous microspheres are obtained by the reaction in heating, is washed with ethyl alcohol aminated
Magnetic porous microspheres 4-5 times are to remove surface impurity.
Further, dry to require to be 1 hour dry under the conditions of 48-52 DEG C in step 3.It is done under this condition
It is dry, it is easy to later stage preservation.
Further, in step 3, the condition saved backup is+4 DEG C.There can be preferable preservation effect under this condition.
Compared with prior art, the present invention advantage is：It can fast and effeciently be prepared by preparation method of the present invention
Provide the nano-scale magnetic iron oxide particle of stronger heavy metal adsorption, and prepared nano-scale magnetic ferriferous oxide
Particle is easy to store spare；The nano-scale magnetic iron oxide particle can carry out the heavy metal in water body quick adsorption, and
It is easily recycled, prevents from causing secondary pollution.
Description of the drawings
Fig. 1 is the preparation method flow chart of the present invention；
Fig. 2 is the transmission electron microscope picture (TEM) of nano-scale magnetic iron oxide particle prepared by the present invention；
Fig. 3 is the infrared spectrum (FTIR) of nano-scale magnetic iron oxide particle prepared by the present invention；
Fig. 4 is the X-ray diffraction spectrogram (XRD) of nano-scale magnetic iron oxide particle prepared by the present invention；
Fig. 5 is the pore-size distribution of nano-scale magnetic iron oxide particle prepared by the present invention.
Specific implementation mode
Technical solution of the present invention is described in detail below in conjunction with the accompanying drawings, but protection scope of the present invention is not limited to
The embodiment.
As shown in Figure 1, the preparation method of aminated magnetic porous microspheres disclosed by the invention, includes the following steps：
Step 1, by FeCl3·6H2O, anhydrous sodium acetate and 1,6- hexamethylene diamines be dissolved in ethylene glycol formed it is transparent molten
Liquid；
Step 2, step 1 gained clear solution is sealed in autoclave, reaction is heated under the conditions of 196-200 DEG C
Obtain aminated magnetic porous microspheres；
Step 3, it is saved backup after drying.
Further, in step 1, used FeCl3·6H2O, anhydrous sodium acetate, 1,6- hexamethylene diamines and ethylene glycol
Amount ratio is 1g：5.6g：3.6g：30mL, for example, by 1.0g FeCl36H2O, 5.6g anhydrous sodium acetates and 3.6g 1,6- oneself
Diamines is dissolved in 30mL ethylene glycol and forms clear solution；It is stirred simultaneously with the speed of agitator of 980-1020rpm in dissolving
It mixes, preferably the speed of agitator of 1000rpm.
Further, in step 2, the heating reaction time in stainless steel autoclave is 4.5-5.5 hours, preferably
It is 5 hours；Used autoclave is the stainless steel autoclave of teflon lined；Preferably in 198 DEG C of items
Reaction is heated under part；After aminated magnetic porous microspheres are obtained by the reaction in heating, aminated magnetic porous microspheres are washed with ethyl alcohol
4-5 times to remove surface impurity.
Further, dry to require to be 1 hour dry under the conditions of 48-52 DEG C in step 3；The condition saved backup be+
4℃。
Embodiment 1：
As shown in Figure 2-5, the obtained aminated magnetic porous microspheres particle crystalline structure of preparation method of the present invention is complete
It is whole, there is good uniformity and consistency, wherein Fig. 2 is the transmission electron microscope of the nano-scale magnetic iron oxide particle prepared
Scheme (TEM), Fig. 3 is the infrared spectrum (FTIR) of the nano-scale magnetic iron oxide particle prepared, and Fig. 4 is the nanoscale magnetic prepared
Property iron oxide particle X-ray diffraction spectrogram (XRD), Fig. 5 is the aperture point of the nano-scale magnetic iron oxide particle prepared
Cloth.
Embodiment 2：
The magnetic Nano iron oxide particle that 0.1g is prepared is dispersed in 100mL deionized waters, using strong
After the external magnetic field that degree is 0.6T recycles 2min, it can realize that the separation of magnetic nanoparticle and water phase, the rate of recovery reach 99.98%
More than.
Embodiment 3：
It is prepared by 0.5g gained aminated magnetic porous microspheres particle be added 100mL, pH value=3.0, Cu it is initial
In the CuCl2 solution of a concentration of 50mg/L, under the conditions of the temperature of 30 DEG C of maintenance, the concussion of 175rpm after reaction 30min, solution
Middle Cu2+Residual concentration be less than 0.05mg/L, meet Cu contents discharge standard in national waste water.
Embodiment 4：
It is prepared by 0.5g gained aminated magnetic porous microspheres particle be added 100mL, pH value=3.0, Zn it is initial
In the ZnCl2 solution of a concentration of 50mg/L, under the conditions of the temperature of 30 DEG C of maintenance, the concussion of 175rpm after reaction 30min, solution
Middle Zn2+Residual concentration be less than 0.12mg/L, meet Zn contents discharge standard in national waste water.
Embodiment 5：
It is prepared by 0.5g gained aminated magnetic porous microspheres particle be added 100mL, pH value=3.0, Cd it is initial
In the CdCl2 solution of a concentration of 50mg/L, under the conditions of the temperature of 30 DEG C of maintenance, the concussion of 175rpm after reaction 30min, solution
Middle Cd2+Residual concentration be less than 0.04mg/L, meet Cd contents discharge standard in national waste water.
Embodiment 6：
It is prepared by 0.5g gained aminated magnetic porous microspheres particle be added 100mL, pH value=3.0, Pb it is initial
In the PbCl2 solution of a concentration of 50mg/L, under the conditions of the temperature of 30 DEG C of maintenance, the concussion of 175rpm after reaction 30min, solution
Middle Pb2+Residual concentration be less than 0.08mg/L, meet Pb contents discharge standard in national waste water.
Embodiment 7：
It is prepared by 0.5g gained aminated magnetic porous microspheres particle be added 100mL, pH value=3.0, Ni it is initial
In the NiCl2 solution of a concentration of 50mg/L, under the conditions of the temperature of 30 DEG C of maintenance, the concussion of 175rpm after reaction 30min, solution
Middle Ni2+Residual concentration be less than 0.05mg/L, meet Ni contents discharge standard in national waste water.
As described above, although the present invention has been indicated and described with reference to specific preferred embodiment, must not explain
For the limitation to invention itself.It without prejudice to the spirit and scope of the invention as defined in the appended claims, can be right
Various changes can be made in the form and details for it.
Claims (9)
1. a kind of preparation method of aminated magnetic porous microspheres, which is characterized in that include the following steps：
Step 1, by FeCl3·6H2O, anhydrous sodium acetate and 1,6- hexamethylene diamines are dissolved in ethylene glycol and form clear solution；
Step 2, step 1 gained clear solution is sealed in autoclave, heats and is obtained by the reaction under the conditions of 196-200 DEG C
Aminated magnetic porous microspheres；
Step 3, it is saved backup after drying.
2. the preparation method of aminated magnetic porous microspheres according to claim 1, which is characterized in that in step 1, made
FeCl3·6H2O, the amount ratio of anhydrous sodium acetate, 1,6- hexamethylene diamines and ethylene glycol is 1g：5.6g：3.6g：30mL.
3. the preparation method of aminated magnetic porous microspheres according to claim 1, which is characterized in that in step 1, molten
Solution is stirred with the speed of agitator of 980-1020rpm simultaneously.
4. the preparation method of aminated magnetic porous microspheres according to claim 1, which is characterized in that in step 2, not
The heating reaction time in rust steel autoclave is 4.5-5.5 hours.
5. the preparation method of aminated magnetic porous microspheres according to claim 1, which is characterized in that in step 2, made
Autoclave is the stainless steel autoclave of teflon lined.
6. the preparation method of aminated magnetic porous microspheres according to claim 1, which is characterized in that in step 2,
Reaction is heated under the conditions of 198 DEG C.
7. the preparation method of aminated magnetic porous microspheres according to claim 1, which is characterized in that in step 2, adding
After thermal response obtains aminated magnetic porous microspheres, it is miscellaneous to remove surface to wash aminated magnetic porous microspheres 4-5 times with ethyl alcohol
Matter.
8. the preparation method of aminated magnetic porous microspheres according to claim 1, which is characterized in that dry in step 3
It is required that be 1 hour dry under the conditions of 48-52 DEG C.
9. the preparation method of aminated magnetic porous microspheres according to claim 1, which is characterized in that in step 3, preserve
Spare condition is+4 DEG C.
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| CN201810496740.7A CN108607514A (en) | 2018-05-22 | 2018-05-22 | A kind of preparation method of aminated magnetic porous microspheres |
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| CN201810496740.7A CN108607514A (en) | 2018-05-22 | 2018-05-22 | A kind of preparation method of aminated magnetic porous microspheres |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102895958A (en) * | 2012-10-24 | 2013-01-30 | 常州大学 | Attapulgite clay based adsorbing material and preparation method thereof |
| CN103041773A (en) * | 2012-12-04 | 2013-04-17 | 天津大学 | Magnetic carbon nanotube composite material and preparation method and application thereof |
| US20130203585A1 (en) * | 2012-02-06 | 2013-08-08 | Korea Institute Of Science And Technology | Composite medium for simultaneous removal of cationic and anionic heavy metals and method for manufacturing the same |
| CN103263886A (en) * | 2013-06-06 | 2013-08-28 | 湖北大学 | Hydrothermal preparation method and application of magnetic ferroferric oxide nanochain |
| CN106745317A (en) * | 2016-11-16 | 2017-05-31 | 杭州电子科技大学 | One-step method prepares method and its application of porous ferroferric oxide magnetic Nano microsphere |
| CN108031440A (en) * | 2017-12-15 | 2018-05-15 | 中国科学院烟台海岸带研究所 | A kind of composite material and its preparation and absorption, remove water body in chromium application |
-
2018
- 2018-05-22 CN CN201810496740.7A patent/CN108607514A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130203585A1 (en) * | 2012-02-06 | 2013-08-08 | Korea Institute Of Science And Technology | Composite medium for simultaneous removal of cationic and anionic heavy metals and method for manufacturing the same |
| CN102895958A (en) * | 2012-10-24 | 2013-01-30 | 常州大学 | Attapulgite clay based adsorbing material and preparation method thereof |
| CN103041773A (en) * | 2012-12-04 | 2013-04-17 | 天津大学 | Magnetic carbon nanotube composite material and preparation method and application thereof |
| CN103263886A (en) * | 2013-06-06 | 2013-08-28 | 湖北大学 | Hydrothermal preparation method and application of magnetic ferroferric oxide nanochain |
| CN106745317A (en) * | 2016-11-16 | 2017-05-31 | 杭州电子科技大学 | One-step method prepares method and its application of porous ferroferric oxide magnetic Nano microsphere |
| CN108031440A (en) * | 2017-12-15 | 2018-05-15 | 中国科学院烟台海岸带研究所 | A kind of composite material and its preparation and absorption, remove water body in chromium application |
Non-Patent Citations (1)
| Title |
|---|
| 金征宇等: "《基因与纳米探针-医学分子成像理论与实践》", 30 November 2017 * |
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