CN110302753A - A kind of preparation method of magnesia-carbon complex microsphere - Google Patents
A kind of preparation method of magnesia-carbon complex microsphere Download PDFInfo
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- CN110302753A CN110302753A CN201910550145.1A CN201910550145A CN110302753A CN 110302753 A CN110302753 A CN 110302753A CN 201910550145 A CN201910550145 A CN 201910550145A CN 110302753 A CN110302753 A CN 110302753A
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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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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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
- B01J20/20—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
- B01J20/28—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
- B01J20/28019—Spherical, ellipsoidal or cylindrical
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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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- 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
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
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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
- C02F2101/20—Heavy metals or heavy metal compounds
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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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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Abstract
The invention belongs to new material technology fields, a kind of preparation method of magnesia-carbon complex microsphere is provided, mainly magnesium salt solution and carbon raw material solution are mixed, precursor solution is configured under stirring condition, precursor solution or colloidal sol are passed through into aerosol generator by carrier gas, reacted into being heated in tube furnace, then is separated gas phase and solid phase by solid-gas separator by carrier gas, magnesia-carbon complex microsphere head product is obtained, and obtains magnesia-carbon complex microsphere after washed calcining.This method have the characteristics that it is easy to operate, without using surfactant, can continuously prepare.The composite microsphere material of preparation has high-specific surface area, not only can heavy metal ion, antibiotic and organic dyestuff in absorption effluent, moreover it is possible to kill bacterium in water.
Description
Technical field
The invention belongs to new material technology fields, and in particular to a kind of preparation method of magnesia-carbon complex microsphere and answer
With.
Background technique
As a kind of important adsorbent, catalyst and anti-biotic material, nano magnesia (MgO) water process, Industrial Catalysis,
The fields such as antibacterial product extensive application.The differences such as sheet, flower-shaped, fibrous are prepared by the thermal decomposition of difference precursor containing magnesium
The nano magnesia of pattern is largely reported.In order to improve the dispersibility and stability of nano magnesia, there are different groups
At magnesium oxide base composite and application performance reported that such as Li-MgO composite construction can be used for methane oxidation coupling successively
It is reacted with oxidative dehydrogenation of ethane, MgO-TiO2Laminated film can be used for gas sensing, and ZnO-MgO composite material is anti-to Linezolid
Raw element has good adsorption property, and MgO coats Ag/TiO2Light can phenol in catalytic degradation water under sunlight for composite material.
Since carbon material has pore structure abundant and bigger serface, magnesia-carbon composite is in adsorbent and urges
Change field has broad application prospects.It has been reported that and hollow sphere is prepared for by the method for electric arc spraying using magnesite ink
MgO-C composite material, before also having been reported that and being using Mg-MOF-74, the mesoporous carbon containing magnesium salts or the biomass containing magnesium salts
Body is driven, blocky, spongiform magnesia-carbon composite is prepared for by the method for dinectly bruning.Many methods there is also at
This height, granule-morphology are irregular, are not easy the problems such as continuously preparing, and also lack simplicity at present and prepare magnesia-carbon complex microsphere
Method.
Summary of the invention
The object of the present invention is to provide a kind of magnesia-carbon complex microsphere preparation method, magnesia-carbon of preparation is compound
Material can be used for water treatment field, especially absorption underwater gold category ion and organic dyestuff.
Technical solution of the present invention:
A kind of preparation method of magnesia-carbon complex microsphere, steps are as follows:
Step 1. mixes magnesium salt solution and carbon raw material solution, is configured to precursor solution under stirring condition；
Step 2. is molten by gas by precursor solution by carrier gas under 10~90 DEG C, 200~500r/min stirring condition
Glue generator enters back into calcination reaction in tube furnace, then is separated gas phase and solid phase by solid-gas separator by carrier gas, and receive
Collection solid powder obtains magnesia-carbon complex microsphere.
It is dry in 60 DEG C of baking oven by magnesia-carbon complex microsphere head product after washing, later in N2Under atmosphere
2h is calcined, magnesia-carbon complex microsphere is obtained.
The molar ratio of the magnesium salts and carbon raw material is 1:0.2~1:2.
The calcination temperature is 400~1000 DEG C.
The magnesium salts be Magnesium dichloride hexahydrate, magnesium nitrate hexahydrate or bitter salt, the magnesium salt solution
Concentration is 0.01~4mol/L；The carbon raw material is glucose, maltose, the formaldehyde of molar ratio 1:0.2~4 and isophthalic two
Phenol, the phenol of molar ratio 1:0.4~4 and formaldehyde or beta-cyclodextrin, the concentration of the carbon raw material solution are 0.01~4mol/
L。
The carrier gas is air, nitrogen or helium.
Compared with prior art, effect and benefit of the invention are as follows: by magnesium salts and carbon raw material mixed aqueous solution or colloidal sol,
Presoma is formed after being atomized using aerosol generator, and using carrier gas continuous calcining easy can to obtain magnesia-carbon compound micro-
Ball, have the characteristics that it is easy to operate, without using surfactant, can continuously prepare.The composite microsphere material of preparation has high ratio
Surface area, not only can heavy metal ion, antibiotic and organic dyestuff in absorption effluent, moreover it is possible to kill bacterium in water.
Detailed description of the invention
Fig. 1 is magnesia-carbon complex microsphere scanning electron microscope diagram of preparation.
Fig. 2 is magnesia-carbon complex microsphere transmission electron microscope figure of preparation.
Fig. 3 is that magnesia-carbon complex microsphere of preparation adsorbs Congo red thermoisopleth.
Fig. 4 is the thermoisopleth of magnesia-carbon complex microsphere absorption Pb (II) of preparation.
Specific embodiment
A specific embodiment of the invention is described below in conjunction with technical solution, but is not limited the scope of the invention.
Embodiment 1
By the 100mL MgCl of 2mol/L2It is mixed with the 100mL glucose solution of 0.5mol/L, passes through stream after mixing evenly
Speed is that 1.0L/min air passes through aerosol generator and tubular type pyrolysis oven, and the temperature of tube furnace is 600 DEG C, is separated by solid gas
Device separates gas phase and solid phase, obtains head product.It is dry in 60 DEG C of baking oven by head product after washing three times, later
In N2It is placed in tube furnace under atmosphere, in 600 DEG C of calcining 2h, obtains magnesia-carbon complex microsphere.Its structure such as Fig. 1 and Fig. 2 institute
Show.
Magnesia-carbon complex microsphere to it is Congo red be representative organic dyestuff and Pb (II) be representative heavy metal ion have
There is good adsorbent performance.100ppm is used respectively, 5min is chosen as test solution in the Congo red of 500ppm, 1000ppm,
10min, 15min, 20min and 25min, as the time point of test, Adsorption experimental results show all to basically reach in 5min
Adsorption equilibrium, the rate of adsorption is very fast, and removal rate is respectively 99.85%, 99.2% and 96.8%, meets pseudo-second-order equation absorption
Model；Absorption, which meets Langmuir model, to be shown to Congo red adsorption isotherm, theoretical adsorption capacity is up to 4024mg/g, such as Fig. 3
It is shown.
It the use of Pb (II) aqueous solution of 1000ppm, 2000ppm, 3000ppm, 4000ppm and 5000ppm is respectively test
Solution, research shows that magnesia-carbon complex microsphere meets Langmuir model to Pb (II) absorption, theoretical adsorption capacity is up to
5166mg/g, as shown in Figure 4.
Magnesia-carbon complex microsphere tetracycline adsorption experiments experiment at 50ppm, in 5min the result shows that basically reach suction
Attached balance, the rate of adsorption is very fast, and removal rate is respectively 95.5%；At 100ppm, adsorption equilibrium is basically reached in 15min, is gone
Except rate is respectively 82.1%.
In addition, antibacterial experiment shows that the complex microsphere of preparation is equal to the antibiotic rate of Escherichia coli and staphylococcus aureus
Greater than 98%.
Embodiment 2
By the 100mLMgCl of 2mol/L2With the resorcinol and formalin (molar ratio 1:2) of the 100mL of 0.5mol/L
Mixing is after mixing evenly aerosol generator and tubular type pyrolysis oven of the 1.5L/min nitrogen by reaction unit by flow velocity,
The temperature of tube furnace is 600 DEG C, separates gas phase and solid phase by solid-gas separator, collects solid powder and obtain head product；It will
The head product being collected into is centrifuged after washing three times, and the solid powder being collected into is dry in 60 DEG C of baking oven, later in N2
Under atmosphere, temperature is that 2h is calcined at 500 DEG C, obtains magnesia-carbon complex microsphere.Magnesia-carbon complex microsphere is to Congo red
The organic dyestuff and Pb (II) of representative are that the heavy metal ion of representative has good adsorbent performance；Antibacterial experiment shows compound micro-
Ball reaches 99% to the antibiotic rate of Escherichia coli and staphylococcus aureus.
Embodiment 3
By the 100mL MgCl of 1mol/L2It is mixed with the 100mL beta-cyclodextrin solution of the 0.1mol/L with hot water dissolving,
It under heating condition after mixing evenly, is aerosol generator and tubular type heat of the 1.5L/min nitrogen by reaction unit by flow velocity
Furnace is solved, and the temperature of tube furnace is 600 DEG C, gas phase and solid phase is separated by solid-gas separator, collects solid powder and obtain primiparity
Product are centrifuged after washing three times, and the solid powder being collected into is dry in 80 DEG C of baking oven, by the product after drying in N2Atmosphere
Under enclosing, temperature is that 2h is calcined at 500 DEG C, obtains magnesia-carbon complex microsphere.The magnesia of preparation-carbon complex microsphere is to the Congo
Red, Pb (II) has good adsorbent performance, and reaches 99% to the antibiotic rate of Escherichia coli and staphylococcus aureus.
Claims (10)
1. a kind of magnesia-carbon complex microsphere preparation method, which is characterized in that steps are as follows:
Step 1. mixes magnesium salt solution and carbon raw material solution, is configured to precursor solution under stirring condition；
Step 2. sends out precursor solution by aerosol under 10~90 DEG C, 200~500r/min stirring condition, through carrier gas
Raw device enters back into calcination reaction in tube furnace, then is separated gas phase and solid phase by solid-gas separator by carrier gas, and collect solid
Body powder obtains magnesia-carbon complex microsphere.
2. preparation method according to claim 1, which is characterized in that by magnesia-carbon complex microsphere after washing,
It is dry in 60 DEG C of baking oven, later in N22h is calcined under atmosphere, obtains magnesia-carbon complex microsphere.
3. preparation method according to claim 1 or 2, which is characterized in that the molar ratio of the magnesium salts and carbon raw material
For 1:0.2~1:2.
4. preparation method according to claim 1 or 2, which is characterized in that the calcination temperature is 400~1000 DEG C.
5. preparation method according to claim 3, which is characterized in that the calcination temperature is 400~1000 DEG C.
6. according to claim 1, preparation method described in 2 or 5, which is characterized in that the magnesium salts is Magnesium dichloride hexahydrate, six
Nitric hydrate magnesium or bitter salt, the concentration of the magnesium salt solution are 0.01~4mol/L；The carbon raw material is
Glucose, maltose, the formaldehyde of molar ratio 1:0.2~4 and resorcinol, the phenol of molar ratio 1:0.4~4 and formaldehyde or β-ring
Dextrin, the concentration of the carbon raw material solution are 0.01~4mol/L.
7. preparation method according to claim 3, which is characterized in that the magnesium salts is Magnesium dichloride hexahydrate, six hydrations
Magnesium nitrate or bitter salt, the concentration of the magnesium salt solution are 0.01~4mol/L；The carbon raw material is grape
Sugar, maltose, the formaldehyde of molar ratio 1:0.2~4 and resorcinol, the phenol of molar ratio 1:0.4~4 and formaldehyde or β-ring paste
Essence, the concentration of the carbon raw material solution are 0.01~4mol/L.
8. the preparation method according to claim 4, which is characterized in that the magnesium salts is Magnesium dichloride hexahydrate, six hydrations
Magnesium nitrate or bitter salt, the concentration of the magnesium salt solution are 0.01~4mol/L；The carbon raw material is grape
Sugar, maltose, the formaldehyde of molar ratio 1:0.2~4 and resorcinol, the phenol of molar ratio 1:0.4~4 and formaldehyde or β-ring paste
Essence, the concentration of the carbon raw material solution are 0.01~4mol/L.
9. according to claim 1, preparation method described in 2,5,7 or 8, which is characterized in that the carrier gas be air, nitrogen or
Helium.
10. preparation method according to claim 6, which is characterized in that the carrier gas is air, nitrogen or helium.
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Cited By (3)
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| CN113244888A (en) * | 2021-05-17 | 2021-08-13 | 内蒙古工业大学 | Modified lignite-based adsorption material and preparation method and application thereof |
| CN114735671A (en) * | 2021-01-07 | 2022-07-12 | 中国石油天然气股份有限公司 | Nitrogen-doped carbon microsphere and preparation method and application thereof |
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| CN114735671B (en) * | 2021-01-07 | 2023-10-31 | 中国石油天然气股份有限公司 | Nitrogen-doped carbon microsphere as well as preparation method and application thereof |
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