CN108455539A - A kind of nano magnesium peroxide and preparation method thereof - Google Patents
A kind of nano magnesium peroxide and preparation method thereof Download PDFInfo
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- CN108455539A CN108455539A CN201810589534.0A CN201810589534A CN108455539A CN 108455539 A CN108455539 A CN 108455539A CN 201810589534 A CN201810589534 A CN 201810589534A CN 108455539 A CN108455539 A CN 108455539A
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/04—Metal peroxides or peroxyhydrates thereof; Metal superoxides; Metal ozonides; Peroxyhydrates thereof
- C01B15/043—Metal peroxides or peroxyhydrates thereof; Metal superoxides; Metal ozonides; Peroxyhydrates thereof of alkali metals, alkaline earth metals or magnesium or beryllium or aluminium
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- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
- C01B25/451—Phosphates containing plural metal, or metal and ammonium containing metal and ammonium
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- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus 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
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Abstract
The invention belongs to solid compound synthesis technical fields, more particularly to a kind of preparation method of nano magnesium peroxide, mainly include the dissolving of magnesium chloride in water, the addition of ammonium hydroxide, PEG200, hydrogen peroxide is titrated, and pH, the centrifugation of suspension are adjusted with NaOH solution, washing, the filtering of deposit, the drying of final product.Invention additionally discloses a kind of nano magnesium peroxides prepared using the preparation method, there is the specific surface area of smaller grain size and bigger using peromag prepared by this method, compared with general commercially available peromag, there is more obvious advantage on phosphorus ligands and dissolving oxygen evolution.
Description
Technical field
The invention belongs to solid compound synthesis technical fields, and in particular to a kind of nano magnesium peroxide and preparation method thereof.
Background technology
Contemporary society, as economic is constantly progressive, industrial, agricultural production to be constantly progressive, various environmental problems are spontaneously
And give birth to, it is increasing for the needs of grain especially with the continuous growth of population, and the grain demand of bigger promotes agricultural
The usage amount of chemical fertilizer gradually increases in production, especially nitrogenous fertilizer, phosphate fertilizer, application it is more.In the fertilizer of application, greatly
It does not fixed, utilize by crop, but hide in the soil, with rainwash and soil erosion.Nutriment in fertilizer
It migrates, is entered eventually into the water bodys such as lake, river therewith.Simultaneously in stain disease caused by human lives, also contain more
The nutriments such as nitrogen, phosphorus.After discharge, some enters in municipal sewage plant these stain diseases, and meeting also is straight
Run in and be put into environment, eventually pass through rainwash, can also converge in the water bodys such as lake, river.
The nutriments such as excessive nitrogen phosphorus have been gathered in water environment, can make the algae in water and phytoplankton large-scale outbreak
Property proliferation, consume the dissolved oxygen in water, keep aquatic animal dead due to anoxic.After algae death simultaneously, corpse decomposes, and will produce
A large amount of nutriment, vicious circle, when dissolved oxygen content is very low, animals and plants remains can carry out anaerobic digestion in water, production
Sulphidisation makes water body color blackening, and generates niff.
Peromag, molecular formula MgO2, it is a kind of solid peroxide, appearance is white powder, tasteless, is insoluble in
Water, is soluble in acid, relatively stable under room temperature, and oxygen can be released under the environment of heating or humidity.Peromag is as one
Kind peroxide, can the effect certain with generation is administered of the prevention to black and odorous water.First, peromag is added to black smelly water
After in body, dissolved oxygen can be discharged in water, dissolved oxygen content is made to increase, and the raising of dissolved oxygen content, be on the one hand conducive to move
On the other hand the existence of object can also hinder the generation of anaerobic reaction, avoid the gas for generating the unpleasant property such as sulfide, can be effective
Prevention black and odorous water generation.In addition to this, peromag can promote the life of guanite as a kind of important magnesium source
At, and the structure of guanite is MgNH4PO4·6H2O can occur coprecipitation reaction with nitrogen, the phosphorus in water, play and effectively go
Except effect.With the reduction of the nutrition contents such as nitrogen phosphorus in dampening, the trend of the explosive proliferation of algae and phytoplankton in water
To be contained, while quantity obtains control, consumption and normal food chain relation to dissolved oxygen will be also maintained,
Avoid the generation of eutrophication.Meanwhile the guanite of generation is also a kind of excellent fertilizer, after collection processing, can be applied
Into soil, the nitrogen and phosphorus element needed for plant growth is provided, promotes plant growth, reduces the use of chemical fertilizer.Phosphorus is used as one kind not
Renewable resource mostlys come from the exploitation and utilization of rock phosphate in powder, and with the large-scale use of chemical fertilizer, phosphor resource is presented
Go out the trend of continuous reduction, if things go on like this, is necessarily faced with exhausted threat.And the utilization of guanite, in going water removal
Nutriment reduces water body load,, will also as a kind of important channel of recycling phosphor resource while preserving the ecological environment
Phosphorus recycling through using and being lost in, utilizes, realizes the benign cycle of phosphor resource, extend the service life of phosphorus again.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of nano magnesium peroxides and preparation method thereof.
The present invention is first technical solution for solving to propose the technical issues of proposition in the prior art：A kind of nanometer of mistake
The preparation method of magnesia, includes the following steps：
1) a certain amount of magnesium chloride will be weighed, will be dissolved into water；
Wherein, the molal weight of water is 40~70 times of magnesium chloride；
2) ammonium hydroxide (1M) is added under stiring and PEG 200 obtains solution；
Wherein, the volume that the volume of ammonium hydroxide is 1/2~2/3, the PEG 200 of the volume of water in the step 1) is the step
It is rapid 1) in 4~6 times of volume of water；
3) 1/2~2/3 hydrogen peroxide that volume is the volume of water in the step 1) is added drop-wise to the step 2) solution
In, it stirs 2~5 hours；
4) pH to 11~11.5 is adjusted with NaOH solution, obtains white suspension；
5) precipitation in white suspension is detached by centrifugal separation, the substance NaOH solution after separation is clear
It washes；
6) it is cleaned with distilled water；
7) it filters, deposit is in drying in oven.
4) and step 6) will carry out under continuous stirring condition, mixing speed 100 step 1) of the present invention is to
~300 rev/min.
Hydrogen peroxide mass concentration is 30~35% in step 3) of the present invention.
Hydrogen peroxide rate of addition is 1~4 drop per minute in step 3) of the present invention.
The pH of NaOH solution is 12~13.5 in step 4) of the present invention.
The rotating speed centrifuged in step 5) of the present invention is 3000~10000 revs/min.
The pH of NaOH solution is 12~13.5 in step 5) of the present invention.
It is 1~5 that NaOH solution wash number is used in step 5) of the present invention.
Number is 3~5 wash with distilled water in step 6) of the present invention.
At 50~80 DEG C, the time is 2~10h for oven temperature control in step 7) of the present invention.
Second technical solution proposed by the present invention is the nano magnesium peroxide prepared using above-mentioned preparation method, average grain
For diameter between 300~500nm, laminar and thickness is only tens nanometers.
Advantageous effect：
In field of environment protection, peromag is a kind of important magnesium source, can be acted on nitrogen phosphorus, generates guanite
(MgNH4PO4·6H2O), it is a kind of effective ways removing nitrogen phosphorus in water removal, is usually used in the improvement of eutrophication water.It is raw simultaneously
At guanite be also a kind of good fertilizer, can be exerted into soil, increase the nutrients such as nitrogen phosphorus in soil, improve soil
pH.Peromag can discharge oxygen compared to magnesium chloride while going to denitrogenate phosphorus, gradually restore the dissolved oxygen in water, molten
The raising for solving oxygen is all highly beneficial for the existence of organism in water and the prevention of black and odorous water and improvement.And it is nano level
Material itself has the specific surface area of smaller grain size and bigger, and dispersibility is more preferable, is conducive to improve reaction efficiency, enhancing is administered
Effect, specifically:
1, the peromag grain size obtained by the present invention will be much smaller than general commercially available peromag, average grain diameter 300-
Between 500nm, and general commercially available peromag grain size is micron or more；Meanwhile according to scanning electron microscope as a result, the invention is made
It is flake to obtain sample, and thickness is only tens nanometers, and peromag is made to have the specific surface area of bigger.
2, the P elements in water body of the sample obtained by the present invention are removed and are dissolved in oxygen evolution, show to be substantially better than
The case where commercially available peromag, illustrates that in the improvement of water body, the peromag obtained by the present invention will will produce better effect
Fruit.
Description of the drawings
Fig. 1 is sample MgO obtained by the present invention2(Nano) XRD results；
Fig. 2 is the scanning electron microscope result of sample obtained by the present invention；
The comparison of two kinds of peromag tp removal rates of Fig. 3；
Fig. 4 is comparison of two kinds of peromags in dissolving oxygen evolution.
Specific implementation mode
Below by specific embodiments and the drawings, the present invention is further illustrated.The embodiment of the present invention is in order to more
So that those skilled in the art is more fully understood the present invention well, any limitation is not made to the present invention.
Embodiment 1
A kind of preparation method of nano magnesium peroxide, includes the following steps：
1) magnesium chloride that will weigh 5.5g is dissolved into 30ml water；
2) 15ml ammonium hydroxide (1M) is added under stiring and 120ml PEG 200 obtain solution, the wherein dosage of ammonium hydroxide is water
The dosage of 1/2, PEG 200 of dosage be 4 times of dosage of water；
3) hydrogen peroxide (mass concentration 30%) that volume is 15ml is added to the speed of 3 drop per minute in solution,
After stirring 2 hours, transparent yellow solution is obtained；
4) NaOH solution of pH=13 is used to adjust pH to 11.5, after NaOH is added, solution has reformed into a kind of hanging for white
Supernatant liquid；
5) (10 points of centrifugation is detached to the precipitation in white suspension by centrifugal separation (6000 revs/min)
Clock), the substance after separation is cleaned 3 times with the NaOH solution of pH=13；
6) it finally, is cleaned, is cleaned 3 times with distilled water；
7) it filters, deposit dries 2h in 80 DEG C of baking oven.
4) and step 6) will carry out under continuous stirring condition for the step 1) to, mixing speed is 100~300
Rev/min.
Sample MgO obtained by the present embodiment2(Nano) the results are shown in Figure 1 by XRD, and the results are shown in Figure 2 for scanning electron microscope.
It can be seen that peromag grain size prepared by the present invention will be much smaller than general commercially available peromag, average grain diameter 300-
Between 500nm, and general commercially available peromag grain size is micron or more；Meanwhile according to scanning electron microscope as a result, the invention is made
It is flake to obtain sample, and thickness is only tens nanometers, and peromag is made to have the specific surface area of bigger.
Embodiment 2
A kind of preparation method of nano magnesium peroxide, includes the following steps：
1) magnesium chloride that will weigh 3g is dissolved into 30ml water；
2) 15ml ammonium hydroxide (1M) is added under stiring and 120ml PEG 200 obtain solution, the wherein dosage of ammonium hydroxide is water
The dosage of 1/2, PEG 200 of dosage be 4 times of dosage of water；
3) hydrogen peroxide (mass concentration 30%) that volume is 15ml is added to the speed of 2 drop per minute in solution,
After stirring 3 hours, transparent yellow solution is obtained；
4) NaOH solution of pH 13.5 is used to adjust pH to 11.3, after NaOH is added, solution has reformed into a kind of hanging for white
Supernatant liquid；
5) (10 points of centrifugation is detached to the precipitation in white suspension by centrifugal separation (8000 revs/min)
Clock), the substance after separation is cleaned 3 times with the NaOH solution of pH 13；
6) it finally, is cleaned, is cleaned 2 times with distilled water；
7) it filters, deposit dries 4h in 80 DEG C of baking oven.
4) and step 6) will carry out under continuous stirring condition for the step 1) to, mixing speed is 100~300
Rev/min.
Embodiment 3
A kind of preparation method of nano magnesium peroxide, includes the following steps：
1) magnesium chloride that will weigh 3g is dissolved into 30ml water；
2) 20ml ammonium hydroxide (1M) is added under stiring and 130ml PEG 200 obtain solution, the wherein dosage of ammonium hydroxide is water
The dosage of 2/3, PEG 200 of dosage be about 4.3 times of dosage of water；
3) hydrogen peroxide (mass concentration 30%) that volume is 20ml is added to the speed of 2 drop per minute in solution,
After stirring 4 hours, transparent yellow solution is obtained；
4) NaOH solution of pH 13 is used to adjust pH to 11, after NaOH is added, solution has reformed into a kind of suspension of white
Liquid；
5) (10 points of centrifugation is detached to the precipitation in white suspension by centrifugal separation (7000 revs/min)
Clock), the substance after separation is cleaned 2 times with the NaOH solution of pH 13；
6) it finally, is cleaned, is cleaned 4 times with distilled water；
7) it filters, deposit dries 2h in 100 DEG C of baking oven.
4) and step 6) will carry out under continuous stirring condition for the step 1) to, mixing speed is 100~300
Rev/min.
Embodiment 4
A kind of preparation method of nano magnesium peroxide, includes the following steps：
1) magnesium chloride that will weigh 2g is dissolved into 20ml water；
2) 10ml ammonium hydroxide (1M) is added under stiring and 100ml PEG 200 obtain solution, the wherein dosage of ammonium hydroxide is water
The dosage of 1/2, PEG 200 of dosage be about 5 times of dosage of water；
3) hydrogen peroxide (mass concentration 30%) that volume is 10ml is added to the speed of 2 drop per minute in solution,
After stirring 2 hours, transparent yellow solution is obtained；
4) NaOH solution of pH 12.5 is used to adjust pH to 11, after NaOH is added, solution becomes a kind of suspension of white
Liquid；
5) (15 points of centrifugation is detached to the precipitation in white suspension by centrifugal separation (7000 revs/min)
Clock), the substance after separation is cleaned 2 times with the NaOH solution of pH 13；
6) it finally, is cleaned, is cleaned 4 times with distilled water；
7) it filters, deposit dries 2h in 100 DEG C of baking oven.
4) and step 6) will carry out under continuous stirring condition for the step 1) to, mixing speed is 100~300
Rev/min.
Embodiment 5
A kind of preparation method of nano magnesium peroxide, includes the following steps：
1) magnesium chloride for weighing 2.5g is dissolved into 30ml water；
2) 20ml ammonium hydroxide (1M) is added under stiring and 120ml PEG 200 obtain solution, the wherein dosage of ammonium hydroxide is water
The dosage of 2/3, PEG 200 of dosage be 4 times of dosage of water；
3) hydrogen peroxide (mass concentration 35%) that volume is 15ml is added to the speed of 3 drop per minute in solution,
After stirring 2 hours, transparent yellow solution is obtained；
4) NaOH solution of pH 13 is used to adjust pH to 11.5, after NaOH is added, solution has reformed into a kind of suspension of white
Liquid；
5) (10 points of centrifugation is detached to the precipitation in white suspension by centrifugal separation (6000 revs/min)
Clock), the substance after separation is cleaned 3 times with the NaOH solution of pH 13；
6) it finally, is cleaned, is cleaned 3 times with distilled water；
7) it filters, deposit dries 2h in 80 DEG C of baking oven.
4) and step 6) will carry out under continuous stirring condition for the step 1) to, mixing speed is 100~300
Rev/min.
Embodiment 6
A kind of preparation method of nano magnesium peroxide, includes the following steps：
1) magnesium chloride for weighing 6g is dissolved into 30ml water (mole of water is 61.66 times of magnesium chloride)；
2) 15ml ammonium hydroxide (1M) is added under stiring and 150ml PEG 200 obtain solution, the wherein dosage of ammonium hydroxide is water
The dosage of 1/2, PEG 200 of dosage be 5 times of dosage of water；
3) hydrogen peroxide (mass concentration 35%) that volume is 15ml is added to the speed of 3 drop per minute in solution,
After stirring 2 hours, transparent yellow solution is obtained；
4) NaOH solution of pH 13.5 is used to adjust pH to 11.5, after NaOH is added, solution has reformed into a kind of hanging for white
Supernatant liquid；
5) (10 points of centrifugation is detached to the precipitation in white suspension by centrifugal separation (8000 revs/min)
Clock), the substance after separation is cleaned 2 times with the NaOH solution of pH 13；
6) it finally, is cleaned, is cleaned 3 times with distilled water；
7) it filters, deposit dries 3h in 80 DEG C of baking oven.
4) and step 6) will carry out under continuous stirring condition for the step 1) to, mixing speed is 100~300
Rev/min.
Embodiment 7
A kind of preparation method of nano magnesium peroxide, includes the following steps：1) magnesium chloride for weighing 4.5g, is dissolved into 30ml
In water；
2) 20ml ammonium hydroxide (1M) is added under stiring and 120ml PEG 200 obtain solution, the wherein dosage of ammonium hydroxide is water
The dosage of 2/3, PEG 200 of dosage be 4 times of dosage of water；
3) hydrogen peroxide (mass concentration 30%) that volume is 15ml is added to the speed of 2 drop per minute in solution,
After stirring 3 hours, transparent yellow solution is obtained；
4) NaOH solution of pH 13.5 is used to adjust pH to 11.5, after NaOH is added, solution has reformed into a kind of hanging for white
Supernatant liquid；
5) (15 points of centrifugation is detached to the precipitation in white suspension by centrifugal separation (6000 revs/min)
Clock), the substance after separation is cleaned 3 times with the NaOH solution of pH 13；
6) it finally, is cleaned, is cleaned 5 times with distilled water；
7) it filters, deposit dries 2h in 80 DEG C of baking oven.
4) and step 6) will carry out under continuous stirring condition for the step 1) to, mixing speed is 100~300
Rev/min.
Embodiment 8
A kind of preparation method of nano magnesium peroxide, includes the following steps：
1) magnesium chloride for weighing 6g is dissolved into 30ml water (mole of water is 61.66 times of magnesium chloride)；
2) 15ml ammonium hydroxide (1M) is added under stiring and 150ml PEG 200 obtain solution, the wherein dosage of ammonium hydroxide is water
The dosage of 1/2, PEG 200 of dosage be 5 times of dosage of water；
3) hydrogen peroxide (mass concentration 35%) that volume is 15ml is added to the speed of 3 drop per minute in solution,
After stirring 2 hours, transparent yellow solution is obtained；
4) NaOH solution of pH 13.5 is used to adjust pH to 11.5, after NaOH is added, solution has reformed into a kind of hanging for white
Supernatant liquid；
5) (10 points of centrifugation is detached to the precipitation in white suspension by centrifugal separation (8000 revs/min)
Clock), the substance after separation is cleaned 2 times with the NaOH solution of pH 13；
6) it finally, is cleaned, is cleaned 3 times with distilled water；
7) it filters, deposit dries 2h in 60 DEG C of baking oven.
4) and step 6) will carry out under continuous stirring condition for the step 1) to, mixing speed is 100~300
Rev/min.
Embodiment 9
A kind of preparation method of nano magnesium peroxide, includes the following steps：
1) magnesium chloride for weighing 5g is dissolved into 30ml water；
2) 15ml ammonium hydroxide (1M) is added under stiring and 150ml PEG 200 obtain solution, the wherein dosage of ammonium hydroxide is water
The dosage of 1/2, PEG 200 of dosage be 5 times of dosage of water；
3) hydrogen peroxide (mass concentration 30%) that volume is 15ml is added to the speed of 1 drop per minute in solution,
After stirring 5 hours, transparent yellow solution is obtained；
4) NaOH solution of pH 13 is used to adjust pH to 11.5, after NaOH is added, solution has reformed into a kind of suspension of white
Liquid；
5) (10 points of centrifugation is detached to the precipitation in white suspension by centrifugal separation (8000 revs/min)
Clock), the substance after separation is cleaned 2 times with the NaOH solution of pH 13；
6) it finally, is cleaned, is cleaned 3 times with distilled water；
7) it filters, deposit dries 2h in 60 DEG C of baking oven.
4) and step 6) will carry out under continuous stirring condition for the step 1) to, mixing speed is 100~300
Rev/min.
Embodiment 10
A kind of preparation method of nano magnesium peroxide, includes the following steps：
1) magnesium chloride for weighing 3.5g is dissolved into 30ml water；
2) 18ml ammonium hydroxide (1M) is added under stiring and 120ml PEG 200 obtain solution, the wherein dosage of ammonium hydroxide is water
The dosage of 3/5, PEG 200 of dosage be 4 times of dosage of water；
3) hydrogen peroxide (mass concentration 35%) that volume is 15ml is added to the speed of 4 drop per minute in solution,
After stirring 2 hours, transparent yellow solution is obtained；
4) NaOH solution of pH 13.5 is used to adjust pH to 11.5, after NaOH is added, solution has reformed into a kind of hanging for white
Supernatant liquid；
5) (10 points of centrifugation is detached to the precipitation in white suspension by centrifugal separation (8000 revs/min)
Clock), the substance after separation is cleaned 2 times with the NaOH solution of pH 13；
6) it finally, is cleaned, is cleaned 2 times with distilled water；
7) it filters, deposit dries 2h in 80 DEG C of baking oven.
4) and step 6) will carry out under continuous stirring condition for the step 1) to, mixing speed is 100~300
Rev/min.
Embodiment 11
A kind of preparation method of nano magnesium peroxide, includes the following steps：
1) magnesium chloride for weighing 3g is dissolved into 30ml water；
2) 15ml ammonium hydroxide (1M) is added under stiring and 120ml PEG 200 obtain solution, the wherein dosage of ammonium hydroxide is water
The dosage of 1/2, PEG 200 of dosage be 5 times of dosage of water；
3) hydrogen peroxide (mass concentration 30%) that volume is 15ml is added to the speed of 1 drop per minute in solution,
After stirring 5 hours, transparent yellow solution is obtained；
4) NaOH solution of pH 12 is used to adjust pH to 11, after NaOH is added, solution has reformed into a kind of suspension of white
Liquid；
5) (10 points of centrifugation is detached to the precipitation in white suspension by centrifugal separation (3000 revs/min)
Clock), the substance after separation is cleaned 1 time with the NaOH solution of pH 13；
6) it finally, is cleaned, is cleaned 3 times with distilled water；
7) it filters, deposit dries 5h in 60 DEG C of baking oven.
4) and step 6) will carry out under continuous stirring condition for the step 1) to, mixing speed is 100~300
Rev/min.
Embodiment 12
A kind of preparation method of nano magnesium peroxide, includes the following steps：
1) magnesium chloride for weighing 6g is dissolved into 30ml water；
2) 20ml ammonium hydroxide (1M) is added under stiring and 180ml PEG 200 obtain solution, the wherein dosage of ammonium hydroxide is water
The dosage of 2/3, PEG 200 of dosage be 6 times of dosage of water；
3) hydrogen peroxide (mass concentration 35%) that volume is 20ml is added to the speed of 1 drop per minute in solution,
After stirring 5 hours, transparent yellow solution is obtained；
4) NaOH solution of pH 13.5 is used to adjust pH to 11.5, after NaOH is added, solution has reformed into a kind of hanging for white
Supernatant liquid；
5) (10 points of centrifugation is detached to the precipitation in white suspension by centrifugal separation (10000 revs/min)
Clock), the substance after separation is cleaned 5 times with the NaOH solution of pH 13.5；
6) it finally, is cleaned, is cleaned 5 times with distilled water；
7) it filters, deposit dries 5h in 80 DEG C of baking oven.
4) and step 6) will carry out under continuous stirring condition for the step 1) to, mixing speed is 100~300
Rev/min.
Comparison uses：
The present invention carries out simulated experiment, disodium hydrogen phosphate and the chlorination that configuration concentration is 0.1M using use for laboratory ultra-pure water
Ammonium salt solution weighs peromag and commercially available peromag prepared by the present invention, is respectively configured as phosphorus, nitrogen source in simulated experiment
The solution of a concentration of 0.1M；And peromag is insoluble in water, so during configuration, the peromag weighed is placed in
It in beaker, after water is added, is positioned on magnetic stirring apparatus, carries out pipetting for peromag under agitation.
Experimental setup system total volume is 100ml, and reactor is two closed screw socket bottles, is added in the reactor first
Then the ultra-pure water of 96ml pipettes the solution containing phosphate of 1ml and contains nitrogen solution, is added in reactor respectively；It is then anti-at two
Answer the peromag solution that 2ml is separately added into device, confined reaction.Due to nitrogen, a concentration of 0.1M of phosphorus, magnesium solution, so always
A concentration of 1mmol/L of nitrogen, phosphorus in system, a concentration of 2mmol/L of magnesium, then at 10 minutes, 25 minutes, 60 minutes and 180
It is sampled when minute, the concentration of phosphorus in measurement system.
Prepare two closed conical flasks simultaneously, nitrogen, phosphorus, magnesium is added according to the above method, but before addition, to reaction
In device lead to nitrogen, oxygen contained in water is discharged, so that dissolved oxygen content is dropped to 0.2mg/L hereinafter, later 10 minutes, 30
Minute, 1 hour, 2 hours, 3 hours, 4 hours, 5 hours, 8 hours, 12 hours and 24 hours carry out the measurement of dissolved oxygen, comparison
Difference of two kinds of peromags in dissolving oxygen evolution.
From figure 3, it can be seen that the MgO prepared through the invention2(Nano) (red line) is much larger than city on tp removal rate
The MgO sold2, for commercially available MgO2, when being 11.9%, 60 minutes when the removal rate of phosphorus is 12.99%, 25 minutes at 10 minutes
It is 18.40% when being 17.32%, 180 minutes；And the MgO for preparing by the method for the invention2(Nano) at 10 minutes,
Tp removal rate has just had reached 40.04%, remote super and commercially available common MgO2, and at 25 minutes, removal rate reaches
Reach 61.69% when 51.95%, 60 minutes, at 180 minutes, has reached 68.18%, than commercially available MgO2Removal rate it is high
More than 3 times.So by data above, it is not difficult to find that the MgO prepared through the invention2(Nano) it is showed on tp removal rate
Go out far above general commercially available MgO2Advantage, be to be advantageous to come into operation, carry out sewage disposal.
As can be seen from Figure 4.In dissolving oxygen evolution, MgO prepared by the present invention2(Nano), in the release of dissolved oxygen speed
It will be slower than commercially available MgO on degree2, the amount of initial dissolution oxygen is 0.2mg/L, and two kinds of MgO are being added2Afterwards, dissolved oxygen starts to become
Change, it can be seen from the figure that the amount of dissolved oxygen is in this period from 0 to 8 day, no matter in which sampled point, system of the present invention
Standby MgO2(Nano) dissolved oxygen discharged will be less than commercially available common MgO2, and in the improvement of black and odorous water, MgO2It is
It is used as a kind of sustained release agent of dissolved oxygen, therefore, MgO prepared by the present invention2(Nano) it is more suitable for the place of water body
During reason.
By comparing above, it can be seen that no matter the peromag prepared by the present invention compares commercially available peromag
It is or on the rate of release of dissolved oxygen, to be all more applicable for the control of water body, therefore in reality in the removal of phosphorus
Sewage disposal in, will also play better treatment effect.
It should be understood that embodiment and example discussed herein simply to illustrate that, to those skilled in the art
For, it can be improved or converted, and all these modifications and variations should all belong to the protection of appended claims of the present invention
Range.
Claims (11)
1. a kind of preparation method of nano magnesium peroxide, which is characterized in that include the following steps：
1) a certain amount of magnesium chloride will be weighed, will be dissolved into water；
Wherein, the molal weight of water is 40~70 times of magnesium chloride；
2) 1M ammonium hydroxide is added under stiring and PEG 200 obtains solution；
Wherein, the volume that the volume of ammonium hydroxide is 1/2~2/3, the PEG 200 of the volume of water in the step 1) is the step 1)
4~6 times of the volume of middle water；
3) 1/2~2/3 hydrogen peroxide that volume is the volume of water in the step 1) is added drop-wise in the step 2) solution, is stirred
It mixes 2~5 hours；
4) pH to 11~11.5 is adjusted with NaOH solution, obtains white suspension；
5) precipitation in white suspension is detached by centrifugal separation, the substance after separation is cleaned with NaOH solution；
6) it is cleaned with distilled water；
7) it filters, deposit is in drying in oven.
2. a kind of preparation method of nano magnesium peroxide according to claim 1, which is characterized in that the step 1) is to 4)
And step 6) will carry out under continuous stirring condition, mixing speed is 100~300 rev/min.
3. a kind of preparation method of nano magnesium peroxide according to claim 1, which is characterized in that double in the step 3)
Oxygen water quality a concentration of 30~35%.
4. a kind of preparation method of nano magnesium peroxide according to claim 1, which is characterized in that double in the step 3)
Oxygen water droplet acceleration is 1~4 drop per minute.
5. a kind of preparation method of nano magnesium peroxide according to claim 1, which is characterized in that in the step 4)
The pH of NaOH solution is 12~13.5.
6. a kind of preparation method of nano magnesium peroxide according to claim 1, which is characterized in that in the step 5) from
The rotating speed of heart separation is 3000~10000 revs/min.
7. a kind of preparation method of nano magnesium peroxide according to claim 1, which is characterized in that in the step 5)
The pH of NaOH solution is 12~13.5.
8. a kind of preparation method of nano magnesium peroxide according to claim 1, which is characterized in that used in the step 5)
NaOH solution wash number is 1~5.
9. a kind of preparation method of nano magnesium peroxide according to claim 1, which is characterized in that used in the step 6)
Distilled water wash number is 3~5.
10. a kind of preparation method of nano magnesium peroxide according to claim 1, which is characterized in that in the step 7)
At 50~80 DEG C, the time is 2~10h for oven temperature control.
11. a kind of nano magnesium peroxide, using preparation method described in claim 1, which is characterized in that average grain diameter 300
~500nm, laminar and thickness is only tens nanometers.
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| CN101613088A (en) * | 2009-07-29 | 2009-12-30 | 中国科学院青海盐湖研究所 | The method of preparing magnesium peroxide by non-emulsion process |
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| CN101613088A (en) * | 2009-07-29 | 2009-12-30 | 中国科学院青海盐湖研究所 | The method of preparing magnesium peroxide by non-emulsion process |
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| CN110040835A (en) * | 2019-03-15 | 2019-07-23 | 天津大学 | Compound spherical magnesium oxide particle of one kind and preparation method thereof |
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Application publication date: 20180828 |