CN108176370A - A kind of preparation method of magnetic gel heavy metal absorbent - Google Patents
A kind of preparation method of magnetic gel heavy metal absorbent Download PDFInfo
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- CN108176370A CN108176370A CN201711398421.4A CN201711398421A CN108176370A CN 108176370 A CN108176370 A CN 108176370A CN 201711398421 A CN201711398421 A CN 201711398421A CN 108176370 A CN108176370 A CN 108176370A
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- 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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- 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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- 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
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- 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
- B01J20/28047—Gels
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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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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
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Abstract
The invention discloses a kind of preparation method of magnetic gel heavy metal absorbent, the preparation method specifically includes following steps：（1）Fe3O4The preparation of magnetic nanometer；（2）The preparation of the magnetic nanometer of sodium alginate package；（3）By step（2）The magnetic nanometer of the sodium alginate package of preparation is resuspended in epoxychloropropane solution, and hyaluronic acid is completely dissolved in aqueous solution, is added to hyaluronic acid solution in the state of stirring in the magnetic nanometer of sodium alginate package of epoxychloropropane resuspension.Adsorbent prepared by the present invention is to Cu, Cr, Pb, Hg, and the preparation method of adsorbent of the present invention is simple, and raw material type is few, environmentally protective, while magnetic action is easy to isolating and purifying for adsorbent.Therefore, the processing of counterweight aqueous metal solution of the present invention has extensive prospect.
Description
Technical field
The invention belongs to water pollution processing technology fields, and in particular to a kind of preparation side of magnetic gel heavy metal absorbent
Method.
Background technology
With the development of global economy and society, environmental pollution getting worse, wherein industrial wastewater are as main environment
Pollution sources are a great problems for perplexing countries in the world for a long time.Heavy metal ion in industrial wastewater have it is strong it is carcinogenic,
Teratogenesis, mutagenic effect constitute health and ecological environment serious threat, therefore strictly control heavy metal wastewater thereby
It pollutes most important.
Traditional process for treating heavy-metal waste water mainly has chemical precipitation method, ion-exchange, membrane separation process etc., these sides
Method is usually in the presence of investment is big, high energy consumption, operating cost are high, is also easy to produce secondary pollution problems, using being restricted.Absorption method is
The pollutant in water is adsorbed using adsorbent, so as to purify the method for waste water, has the characteristics that easy to operate, fast and effective, obtains
To being widely applied.How to obtain that cheap, adsorption capacity is strong, adsorptive selectivity is high, the suction of environmentally protective, easily separated purifying
Attached dose, have become the hot spot of research and development.
Invention content
In order to of the existing technology more than solving the problems, such as, the purpose of the present invention is to provide a kind of environment-friendly type metals
Cutting fluid and preparation method thereof.
To achieve these goals, the present invention provides following technical scheme：
A kind of preparation method of magnetic gel heavy metal absorbent, the preparation method specifically include following steps：
（1）Fe3O4The preparation of magnetic nanometer
（2）To step（1）The Fe of preparation3O4Glutaraldehyde solution is added in magnetic nanometer so that the final concentration of glutaraldehyde solution
For 0.5-1M, magnetic nanometer is stirred；
（3）Sodium alginate is dissolved with acetic acid to obtain sodium alginate soln, by sodium alginate soln in the state of stirring
It is added to step（2）In magnetic nanometer in, be to slowly warm up to 35-40 DEG C, continue to be stirred to react 2-4h, by being made after centrifugation
Obtain the magnetic nanometer of sodium alginate package；
（4）By step（3）The magnetic nanometer of the sodium alginate package of preparation is resuspended in epoxychloropropane solution, by hyalomitome
Acid is completely dissolved in aqueous solution, and hyaluronic acid solution is added to the alginic acid of epoxychloropropane resuspension in the state of stirring
In the magnetic nanometer of sodium package, 45-60 DEG C is to slowly warm up to, continues to be stirred to react 5-10h, by the way that precipitation is collected by centrifugation, made
It is washed with distilled water 3-5 times, is dried in 50-60 DEG C of baking oven to get magnetic gel heavy metal absorbent.
A kind of preparation method of magnetic gel heavy metal absorbent of the present invention, the specific steps of the preparation method
It is as follows：
（1）Fe3O4The preparation of magnetic nanometer
Fe is prepared using microemulsion method3O4Magnetic nanometer, and magnetic nanometer is dried in an oven；
（2）Weigh 20-50mg steps（1）The Fe of preparation3O4Magnetic nanometer, with the aqueous solution of 10-20mL by magnetic nanometer
Be resuspended and be placed in ultrasonic disperse 10-20min in Ultrasound Instrument, then add in glutaraldehyde solution thereto, glutaraldehyde solution
Final concentration of 0.5-1M, at room temperature stirs magnetic nanometer；
（3）Weigh 15-30mg sodium alginates and be 10-20% with 10-20mL volumetric concentrations acetic acid carry out fully dissolve obtain sea
Sodium alginate soln is added to step by solution of sodium alginate under the rotating speed of 300-500r/min（2）In magnetic nanometer in,
35-40 DEG C is to slowly warm up to, continues to be stirred to react 2-4h, the magnetic nanometer of sodium alginate package is made after reactant is centrifuged
Particle；
（4）By step（3）It is 5-10%'s that the magnetic nanometer of the sodium alginate package of preparation, which is resuspended in 20-30mL volumetric concentrations,
In epoxychloropropane solution, weigh 20-30mg hyaluronic acids and be completely dissolved in aqueous solution, under the rotating speed of 200-300r/min
Hyaluronic acid solution is added in the magnetic nanometer of sodium alginate package of epoxychloropropane resuspension, is to slowly warm up to 45-
60 DEG C, continue to be stirred to react 5-10h, precipitation is collected by centrifugation in reaction system, makes to be washed with distilled water 3-5 times, sediment is put
It is dried in 50-60 DEG C of baking oven to get magnetic gel heavy metal absorbent.
Preferably, the grain size of the magnetic nanometer is 50-100nm.
Preferably, the step（2）Middle Fe3O4The quality of magnetic nanometer be 35mg, the step（3）Middle sodium alginate
Quality for 25mg, the step（4）The quality of middle hyaluronic acid is 25mg.
Preferably, the step（4）The volumetric concentration of middle epoxychloropropane is 8%.
Magnetic gel heavy metal absorbent made from preparation method of the present invention.
Advantageous effect：The invention discloses a kind of preparation method of magnetic gel heavy metal absorbent, with magnetic nanometer
For separating medium, by the cladding of sodium alginate and hyaluronic acid, prepare and have to Cu, Cr, Pb, Hg these types heavy metal ion
There is the magnetic gel adsorbent of stronger suction-operated, more than 100mg/g, present invention absorption are reached to the adsorbance of heavy metal ion
The preparation method of agent is simple, and raw material type is few, environmentally protective, while magnetic action is easy to isolating and purifying for adsorbent.Therefore, originally
The processing of invention counterweight aqueous metal solution has extensive prospect.
Specific embodiment
The invention will now be further described with reference to specific embodiments, but embodiment is only exemplary, not to this hair
Bright range forms any restrictions.It will be understood by those skilled in the art that without departing from the spirit and scope of the invention
Can the details and form of technical solution of the present invention be modified or be replaced, but these modifications and replacement each fall within the present invention's
In protection domain.
Embodiment 1
A kind of preparation method of magnetic gel heavy metal absorbent, the preparation method are as follows：
（1）Fe3O4The preparation of magnetic nanometer
Fe is prepared using microemulsion method3O4Magnetic nanometer, and magnetic nanometer is dried in an oven；
（2）Weigh 35mg steps（1）The Fe of preparation3O4Magnetic nanometer is carried out weight by magnetic nanometer with the aqueous solution of 15mL
It is outstanding to be placed in ultrasonic disperse 15min in Ultrasound Instrument, then add in glutaraldehyde solution thereto, glutaraldehyde solution it is final concentration of
0.8M at room temperature stirs magnetic nanometer；
（3）It weighs 22mg sodium alginates and carries out fully dissolving with the acetic acid that 15mL volumetric concentrations are 15% to obtain sodium alginate molten
Sodium alginate soln is added to step by liquid under the rotating speed of 400r/min（2）In magnetic nanometer in, be to slowly warm up to 37
DEG C, continue to be stirred to react 3h, the magnetic nanometer of sodium alginate package is made after reactant is centrifuged；
（4）By step（3）The magnetic nanometer of the sodium alginate package of preparation is resuspended in the epoxy chlorine that 25mL volumetric concentrations are 8%
In propane solution, weigh 25mg hyaluronic acids and be completely dissolved in aqueous solution, it is under the rotating speed of 250r/min that hyaluronic acid is molten
Liquid is added in the magnetic nanometer of sodium alginate package of epoxychloropropane resuspension, is to slowly warm up to 50 DEG C, and it is anti-to continue stirring
8h is answered, precipitation is collected by centrifugation in reaction system, makes to be washed with distilled water 3-5 times, puts the precipitate in 50-60 DEG C of baking oven and does
It is dry to get magnetic gel heavy metal absorbent.
Preferably, the grain size of the magnetic nanometer is 80nm.
Embodiment 2
A kind of preparation method of magnetic gel heavy metal absorbent, the preparation method are as follows：
（1）Fe3O4The preparation of magnetic nanometer
Fe is prepared using microemulsion method3O4Magnetic nanometer, and magnetic nanometer is dried in an oven；
（2）Weigh 20mg steps（1）The Fe of preparation3O4Magnetic nanometer is carried out weight by magnetic nanometer with the aqueous solution of 10mL
It is outstanding to be placed in ultrasonic disperse 10min in Ultrasound Instrument, then add in glutaraldehyde solution thereto, glutaraldehyde solution it is final concentration of
0.5M at room temperature stirs magnetic nanometer；
（3）It weighs 15mg sodium alginates and carries out fully dissolving with the acetic acid that 10mL volumetric concentrations are 10% to obtain sodium alginate molten
Sodium alginate soln is added to step by liquid under the rotating speed of 300r/min（2）In magnetic nanometer in, be to slowly warm up to 35
DEG C, continue to be stirred to react 2h, the magnetic nanometer of sodium alginate package is made after reactant is centrifuged；
（4）By step（3）The magnetic nanometer of the sodium alginate package of preparation is resuspended in the epoxy chlorine that 20mL volumetric concentrations are 5%
In propane solution, weigh 20mg hyaluronic acids and be completely dissolved in aqueous solution, it is under the rotating speed of 200r/min that hyaluronic acid is molten
Liquid is added in the magnetic nanometer of sodium alginate package of epoxychloropropane resuspension, is to slowly warm up to 45 DEG C, and it is anti-to continue stirring
5h is answered, precipitation is collected by centrifugation in reaction system, makes to be washed with distilled water 3-5 times, puts the precipitate in 50-60 DEG C of baking oven and does
It is dry to get magnetic gel heavy metal absorbent.
Preferably, the grain size of the magnetic nanometer is 50nm.
Embodiment 3
A kind of preparation method of magnetic gel heavy metal absorbent, the preparation method are as follows：
（1）Fe3O4The preparation of magnetic nanometer
Fe is prepared using microemulsion method3O4Magnetic nanometer, and magnetic nanometer is dried in an oven；
（2）Weigh 50mg steps（1）The Fe of preparation3O4Magnetic nanometer is carried out weight by magnetic nanometer with the aqueous solution of 20mL
It is outstanding to be placed in ultrasonic disperse 20min in Ultrasound Instrument, then add in glutaraldehyde solution thereto, glutaraldehyde solution it is final concentration of
1M at room temperature stirs magnetic nanometer；
（3）It weighs 30mg sodium alginates and carries out fully dissolving with the acetic acid that 20mL volumetric concentrations are 20% to obtain sodium alginate molten
Sodium alginate soln is added to step by liquid under the rotating speed of 500r/min（2）In magnetic nanometer in, be to slowly warm up to 40
DEG C, continue to be stirred to react 4h, the magnetic nanometer of sodium alginate package is made after reactant is centrifuged；
（4）By step（3）The magnetic nanometer of the sodium alginate package of preparation is resuspended in the epoxy chlorine that 30mL volumetric concentrations are 10%
In propane solution, weigh 30mg hyaluronic acids and be completely dissolved in aqueous solution, it is under the rotating speed of 300r/min that hyaluronic acid is molten
Liquid is added in the magnetic nanometer of sodium alginate package of epoxychloropropane resuspension, is to slowly warm up to 60 DEG C, and it is anti-to continue stirring
10h is answered, precipitation is collected by centrifugation in reaction system, makes to be washed with distilled water 3-5 times, puts the precipitate in 50-60 DEG C of baking oven and does
It is dry to get magnetic gel heavy metal absorbent.
Preferably, the grain size of the magnetic nanometer is 100nm.
Embodiment 4
A kind of preparation method of magnetic gel heavy metal absorbent, the preparation method are as follows：
（1）Fe3O4The preparation of magnetic nanometer
Fe is prepared using microemulsion method3O4Magnetic nanometer, and magnetic nanometer is dried in an oven；
（2）Weigh 30mg steps（1）The Fe of preparation3O4Magnetic nanometer is carried out weight by magnetic nanometer with the aqueous solution of 12mL
It is outstanding to be placed in ultrasonic disperse 12min in Ultrasound Instrument, then add in glutaraldehyde solution thereto, glutaraldehyde solution it is final concentration of
0.6M at room temperature stirs magnetic nanometer；
（3）It weighs 18mg sodium alginates and carries out fully dissolving with the acetic acid that 12mL volumetric concentrations are 13% to obtain sodium alginate molten
Sodium alginate soln is added to step by liquid under the rotating speed of 350r/min（2）In magnetic nanometer in, be to slowly warm up to 36
DEG C, continue to be stirred to react 2.5h, the magnetic nanometer of sodium alginate package is made after reactant is centrifuged；
（4）By step（3）The magnetic nanometer of the sodium alginate package of preparation is resuspended in the epoxy chlorine that 22mL volumetric concentrations are 6%
In propane solution, weigh 22mg hyaluronic acids and be completely dissolved in aqueous solution, it is under the rotating speed of 230r/min that hyaluronic acid is molten
Liquid is added in the magnetic nanometer of sodium alginate package of epoxychloropropane resuspension, is to slowly warm up to 50 DEG C, and it is anti-to continue stirring
6h is answered, precipitation is collected by centrifugation in reaction system, makes to be washed with distilled water 3-5 times, puts the precipitate in 50-60 DEG C of baking oven and does
It is dry to get magnetic gel heavy metal absorbent.
Preferably, the grain size of the magnetic nanometer is 60nm.
Comparative example 1
A kind of preparation method of magnetic gel heavy metal absorbent, the preparation method are as follows：
（1）Fe3O4The preparation of magnetic nanometer
Fe is prepared using microemulsion method3O4Magnetic nanometer, and magnetic nanometer is dried in an oven；
（2）Magnetic nanometer is resuspended in the epoxychloropropane solution that 25mL volumetric concentrations are 8%, weighs 25mg hyaluronic acids
It is completely dissolved, hyaluronic acid solution is added in magnetic nanometer in aqueous solution under the rotating speed of 250r/min, slowly rise
Temperature continues to be stirred to react 8h to 50 DEG C, and reaction system is collected by centrifugation precipitation, makes to be washed with distilled water 3-5 times, sediment is put
It is dried in 50-60 DEG C of baking oven to get magnetic gel heavy metal absorbent.
Preferably, the grain size of the magnetic nanometer is 80nm.
Comparative example 2
A kind of preparation method of magnetic gel heavy metal absorbent, the preparation method are as follows：
（1）Fe3O4The preparation of magnetic nanometer
Fe is prepared using microemulsion method3O4Magnetic nanometer, and magnetic nanometer is dried in an oven；
（2）Weigh 35mg steps（1）The Fe of preparation3O4Magnetic nanometer is carried out weight by magnetic nanometer with the aqueous solution of 15mL
It is outstanding to be placed in ultrasonic disperse 15min in Ultrasound Instrument, then add in glutaraldehyde solution thereto, glutaraldehyde solution it is final concentration of
0.8M at room temperature stirs magnetic nanometer；
（3）It weighs 22mg sodium alginates and carries out fully dissolving with the acetic acid that 15mL volumetric concentrations are 15% to obtain sodium alginate molten
Sodium alginate soln is added to step by liquid under the rotating speed of 400r/min（2）In magnetic nanometer in, be to slowly warm up to 37
DEG C, continue to be stirred to react 3h, the magnetic nanometer that sodium alginate package is made is dried after reactant is centrifuged.
Preferably, the grain size of the magnetic nanometer is 80nm.
Each 100mg of adsorbent prepared by Example 1-4 and comparative example 1-2, be added to 500mL contains heavy metal ion
Aqueous solution in, the concentration of heavy metal ion Cu, Cr, Pb, Hg are 50mg/mL, at 25 DEG C adsorb 1h after, pass through Magneto separate
Adsorbent is removed, the concentration of heavy metal ion in aqueous solution is detected using HPLC-MS and calculates adsorbance, specific detection data
As shown in table 1：
Table 1
Claims (6)
1. a kind of preparation method of magnetic gel heavy metal absorbent, which is characterized in that the preparation method specifically includes following
Step：
（1）Fe3O4The preparation of magnetic nanometer；
（2）To step（1）The Fe of preparation3O4Glutaraldehyde solution is added in magnetic nanometer so that glutaraldehyde solution it is final concentration of
0.5-1M stirs magnetic nanometer；
（3）Sodium alginate is dissolved with acetic acid to obtain sodium alginate soln, by sodium alginate soln in the state of stirring
It is added to step（2）In magnetic nanometer in, be to slowly warm up to 35-40 DEG C, continue to be stirred to react 2-4h, by being made after centrifugation
Obtain the magnetic nanometer of sodium alginate package；
（4）By step（3）The magnetic nanometer of the sodium alginate package of preparation is resuspended in epoxychloropropane solution, by hyalomitome
Acid is completely dissolved in aqueous solution, and hyaluronic acid solution is added to the alginic acid of epoxychloropropane resuspension in the state of stirring
In the magnetic nanometer of sodium package, 45-60 DEG C is to slowly warm up to, continues to be stirred to react 5-10h, by the way that precipitation is collected by centrifugation, made
It is washed with distilled water 3-5 times, is dried in 50-60 DEG C of baking oven to get magnetic gel heavy metal absorbent.
A kind of 2. preparation method of magnetic gel heavy metal absorbent according to claim 1, which is characterized in that the system
Preparation Method is as follows：
（1）Fe3O4The preparation of magnetic nanometer
Fe is prepared using microemulsion method3O4Magnetic nanometer, and magnetic nanometer is dried in an oven；
（2）Weigh 20-50mg steps（1）The Fe of preparation3O4Magnetic nanometer, with the aqueous solution of 10-20mL by magnetic nanometer into
Row is resuspended and is placed in ultrasonic disperse 10-20min in Ultrasound Instrument, then adds in glutaraldehyde solution, the end of glutaraldehyde solution thereto
A concentration of 0.5-1M, at room temperature stirs magnetic nanometer；
（3）Weigh 15-30mg sodium alginates and be 10-20% with 10-20mL volumetric concentrations acetic acid carry out fully dissolve obtain sea
Sodium alginate soln is added to step by solution of sodium alginate under the rotating speed of 300-500r/min（2）In magnetic nanometer in,
35-40 DEG C is to slowly warm up to, continues to be stirred to react 2-4h, the magnetic nanometer of sodium alginate package is made after reactant is centrifuged
Particle；
（4）By step（3）It is 5-10%'s that the magnetic nanometer of the sodium alginate package of preparation, which is resuspended in 20-30mL volumetric concentrations,
In epoxychloropropane solution, weigh 20-30mg hyaluronic acids and be completely dissolved in aqueous solution, under the rotating speed of 200-300r/min
Hyaluronic acid solution is added in the magnetic nanometer of sodium alginate package of epoxychloropropane resuspension, is to slowly warm up to 45-
60 DEG C, continue to be stirred to react 5-10h, precipitation is collected by centrifugation in reaction system, makes to be washed with distilled water 3-5 times, sediment is put
It is dried in 50-60 DEG C of baking oven to get magnetic gel heavy metal absorbent.
A kind of 3. preparation method of magnetic gel heavy metal absorbent according to claim 1 or 2, which is characterized in that institute
The grain size for stating magnetic nanometer is 50-100nm.
A kind of 4. preparation method of magnetic gel heavy metal absorbent according to claim 2, which is characterized in that the step
Suddenly（2）Middle Fe3O4The quality of magnetic nanometer be 35mg, the step（3）The quality of middle sodium alginate be 25mg, the step
（4）The quality of middle hyaluronic acid is 25mg.
A kind of 5. preparation method of magnetic gel heavy metal absorbent according to claim 2, which is characterized in that the step
Suddenly（4）The volumetric concentration of middle epoxychloropropane is 8%.
6. magnetic gel heavy metal absorbent made from preparation method described in claim 1.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109758989A (en) * | 2019-03-08 | 2019-05-17 | 南京青柠生物科技有限公司 | It is a kind of for purifying the preparation method of the nanometer magnetic bead of histidine tagged protein matter |
| CN110246641A (en) * | 2019-05-05 | 2019-09-17 | 桂林理工大学 | A method of preparing the hyaluronic acid decorated Superparamagnetic Iron Oxide nanoparticle of the degradation of good dispersion |
| CN113797898A (en) * | 2021-10-18 | 2021-12-17 | 青岛理工大学 | Preparation method and application of magnetic adsorbent for efficiently removing elemental mercury and hydrogen sulfide |
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| CN113797898A (en) * | 2021-10-18 | 2021-12-17 | 青岛理工大学 | Preparation method and application of magnetic adsorbent for efficiently removing elemental mercury and hydrogen sulfide |
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