CN109292800A - A kind of Mgo Nanopowder preparation method - Google Patents
A kind of Mgo Nanopowder preparation method Download PDFInfo
- Publication number
- CN109292800A CN109292800A CN201811341331.6A CN201811341331A CN109292800A CN 109292800 A CN109292800 A CN 109292800A CN 201811341331 A CN201811341331 A CN 201811341331A CN 109292800 A CN109292800 A CN 109292800A
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- Prior art keywords
- combustion chamber
- magnesium
- magnesium acetate
- acetic anhydride
- combustion
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Abstract
The invention discloses a kind of Mgo Nanopowder preparation methods, comprising: step 1. dries magnesium acetate 3~5 hours under the conditions of 100 DEG C of temperature, removes the crystallization water;Acetic anhydride magnesium is dissolved in dehydrated alcohol by step 2. with the ratio of 0.1~50:100, forms uniform and stable magnesium acetate solution;By magnesium acetate solution, continuously atomization sprays step 3. in the combustion chamber, while being passed through combustion-supporting gas in the combustion chamber;To burn indoor substance successively-ignited, obtain burning powder;Step 4. collects burning powder;By the burning powder being collected into temperature condition roasted oreization 1~3 hour of 400~800 DEG C in Muffle furnace;The good powder of mineralising is cooled to room temperature to get Mgo Nanopowder by step 5..The active higher, particle size distribution of Mgo Nanopowder produced by the present invention uniformly, good dispersion the features such as, quality is high, and the present invention is suitble to enterprise scale production, good economy performance.
Description
Technical field
The present invention relates to inorganic material, the preparation method of specifically a kind of Mgo Nanopowder.
Background technique
For nano magnesia as a kind of novel and multifunctional inorganic material, particle size compares table between 1~100nm
Area is big, and surface-active is larger, shows the characteristics such as skin effect, bulk effect and quantum tunneling effect.Due to nano oxidized
Magnesium catalysis, optics, magnetics, in terms of shown many special excellent functions, thus there is very important answer
With value, in recent years, having started the research boom of nano oxidized magnesium material in the industry.
Nano magnesia is obtained by what Mgo Nanopowder was realized.Currently, the preparation of Mgo Nanopowder
It is mainly realized with sol-gal process, the although activity with higher of Mgo Nanopowder made from this preparation method, but
It is that due to the low efficiency of the preparation method and the particle size distribution of obtained Mgo Nanopowder is uneven, obtained by it
Nano magnesia inferior quality can only be used as laboratory to be not suitable for large-scale production.It is apparent that this status is very big
The commercial of nano magnesia that limit promote.
Summary of the invention
Technical purpose of the invention is: in view of the above shortcomings of the prior art, bitter earth nano can be made by providing one kind
Powder can obtain greater activity, and can obtain uniform particle size distribution with high efficiency, good dispersion, be suitble to large-scale production
Mgo Nanopowder preparation method.
The present invention realizes its technical purpose the technical scheme adopted is that a kind of Mgo Nanopowder preparation method, institute
Stating preparation method includes following process steps:
Step 1. dries magnesium acetate 3~5 hours under the conditions of 100 DEG C of temperature, removes the crystallization water;
Acetic anhydride magnesium is dissolved in dehydrated alcohol by step 2., and the dissolving ratio of acetic anhydride magnesium and dehydrated alcohol is 0.1~
50:100 forms uniform and stable magnesium acetate solution;
By magnesium acetate solution, continuously atomization sprays step 3. in the combustion chamber, while being passed through combustion-supporting gas in the combustion chamber;It will combustion
Indoor substance successively-ignited is burnt, burning powder is obtained;
Step 4. collects burning powder;
By the burning powder being collected into temperature condition roasted oreization 1~3 hour of 400~800 DEG C in Muffle furnace;
The good powder of mineralising in Muffle furnace is cooled to room temperature to get Mgo Nanopowder by step 5..
One of preferably, acetic anhydride magnesium described in step 2 is in the course of dissolution in dehydrated alcohol, described
Glacial acetic acid is added in dehydrated alcohol to promote dissolution of the acetic anhydride magnesium in dehydrated alcohol, the additional amount of the glacial acetic acid is nothing
The 5~10% of the magnesia amount of water acetic acid.
One of preferably, the concentration of magnesium acetate solution described in step 2 is 0.01mol/L to saturated solution.
One of preferably, the flow that magnesium acetate solution described in step 3 is continuously atomized ejection in the combustion chamber is
10~30mL/min;The flow that the combustion-supporting gas is passed through in the combustion chamber is 15~50L/min.
One of preferably, combustion-supporting gas described in step 3 is for purity oxygen or through the diluted oxygen of nitrogen.
One of preferably, combustion chamber described in step 3 is non-tight type combustion chamber.
The method have the benefit that:
1. the present invention using magnesium acetate as main material, using dehydrated alcohol as solvent, magnesia is prepared by flame combustion process and is received
Rice flour body, Mgo Nanopowder obtained after mineralising is handled active higher, particle size distribution uniformly, the oxygen of good dispersion
Change magnesium nano-powder finished product, which applies crystallinity with higher, parts list in piece surface processing
Face quality is high, and quality is good;Whole preparation process of the invention is simple and easy, convenience and high-efficiency, can be realized and is prepared on a large scale, and is suitble to
Enterprise scale production, good economy performance;
2. the present invention can effectively facilitate acetic anhydride magnesium in dehydrated alcohol during the preparation process by the addition of glacial acetic acid
Solution rate and dissolution quality, make magnesium acetate solution with high efficiency realize uniform stabilization;
3. the continuous atomization of magnesium acetate solution of the present invention in the combustion chamber sprays burning measure, not only there is high efficiency, but also can obtain
Obtain fine and close, uniform Mgo Nanopowder first product, it can be ensured that subsequent mineralising processing is reliably realized with high-quality.
Specific embodiment
The present invention relates to inorganic material, the preparation method of specifically a kind of Mgo Nanopowder, below with multiple implementations
Technology contents of the invention are described in detail in example.
Embodiment 1
The present invention includes following process steps:
Step 1. dries magnesium acetate about 5 hours under the conditions of about 100 DEG C of temperature, removes the crystallization water;
Acetic anhydride magnesium is dissolved in dehydrated alcohol by step 2., and the dissolving ratio of acetic anhydride magnesium and dehydrated alcohol is about
1.42:100;
In course of dissolution, glacial acetic acid is added into dehydrated alcohol, the additional amount of glacial acetic acid is about the 5% of the magnesia amount of acetic anhydride,
Promote solution rate and dissolution quality of the acetic anhydride magnesium in dehydrated alcohol with glacial acetic acid, it is molten to form uniform and stable magnesium acetate
Liquid, the concentration of magnesium acetate solution are about 0.1mol/L;
Step 3. is using non-tight type combustion chamber as combustion chamber;
By magnesium acetate solution, continuously atomization sprays in the combustion chamber, and magnesium acetate solution is continuously atomized the flow of ejection in the combustion chamber
About 30mL/min;
Meanwhile it being passed through combustion-supporting gas in the combustion chamber, which is purity oxygen, the stream that combustion-supporting gas is passed through in the combustion chamber
Amount is about 45L/min;
To burn indoor substance successively-ignited, obtain burning powder;
Step 4. collects burning powder;
By the burning powder being collected into temperature condition roasted oreization about 1 hour of about 800 DEG C in Muffle furnace;
The good powder of mineralising in Muffle furnace is cooled to room temperature to get Mgo Nanopowder by step 5..
Embodiment 2
The present invention includes following process steps:
Step 1. dries magnesium acetate about 4.5 hours under the conditions of about 100 DEG C of temperature, removes the crystallization water;
Acetic anhydride magnesium is dissolved in dehydrated alcohol by step 2., and the dissolving ratio of acetic anhydride magnesium and dehydrated alcohol is about
0.142:100;
In course of dissolution, glacial acetic acid is added into dehydrated alcohol, the additional amount of glacial acetic acid is about the 5% of the magnesia amount of acetic anhydride,
Promote solution rate and dissolution quality of the acetic anhydride magnesium in dehydrated alcohol with glacial acetic acid, it is molten to form uniform and stable magnesium acetate
Liquid, the concentration of magnesium acetate solution are about 0.01mol/L;
Step 3. is using non-tight type combustion chamber as combustion chamber;
By magnesium acetate solution, continuously atomization sprays in the combustion chamber, and magnesium acetate solution is continuously atomized the flow of ejection in the combustion chamber
About 30mL/min;
Meanwhile it being passed through combustion-supporting gas in the combustion chamber, which is purity oxygen, the stream that combustion-supporting gas is passed through in the combustion chamber
Amount is about 45L/min;
To burn indoor substance successively-ignited, obtain burning powder;
Step 4. collects burning powder;
By the burning powder being collected into temperature condition roasted oreization about 1 hour of about 750 DEG C in Muffle furnace;
The good powder of mineralising in Muffle furnace is cooled to room temperature to get Mgo Nanopowder by step 5..
Embodiment 3
The present invention includes following process steps:
Step 1. dries magnesium acetate about 4 hours under the conditions of about 100 DEG C of temperature, removes the crystallization water;
Acetic anhydride magnesium is dissolved in dehydrated alcohol by step 2., and the dissolving ratio of acetic anhydride magnesium and dehydrated alcohol is about
0.71:100;
In course of dissolution, glacial acetic acid is added into dehydrated alcohol, the additional amount of glacial acetic acid is about the 7% of the magnesia amount of acetic anhydride,
Promote solution rate and dissolution quality of the acetic anhydride magnesium in dehydrated alcohol with glacial acetic acid, it is molten to form uniform and stable magnesium acetate
Liquid, the concentration of magnesium acetate solution are about 0.5mol/L;
Step 3. is using non-tight type combustion chamber as combustion chamber;
By magnesium acetate solution, continuously atomization sprays in the combustion chamber, and magnesium acetate solution is continuously atomized the flow of ejection in the combustion chamber
About 25mL/min;
Meanwhile it being passed through combustion-supporting gas in the combustion chamber, which is through the diluted oxygen of 20% nitrogen, and combustion-supporting gas is firing
Burning the indoor flow being passed through is about 46.8L/min;
To burn indoor substance successively-ignited, obtain burning powder;
Step 4. collects burning powder;
By the burning powder being collected into temperature condition roasted oreization about 2 hours of about 700 DEG C in Muffle furnace;
The good powder of mineralising in Muffle furnace is cooled to room temperature to get Mgo Nanopowder by step 5..
Embodiment 4
The present invention includes following process steps:
Step 1. dries magnesium acetate about 3 hours under the conditions of about 100 DEG C of temperature, removes the crystallization water;
Acetic anhydride magnesium is dissolved in dehydrated alcohol by step 2., and the dissolving ratio of acetic anhydride magnesium and dehydrated alcohol is about
0.426:100;
In course of dissolution, glacial acetic acid is added into dehydrated alcohol, the additional amount of glacial acetic acid is about the 6% of the magnesia amount of acetic anhydride,
Promote solution rate and dissolution quality of the acetic anhydride magnesium in dehydrated alcohol with glacial acetic acid, it is molten to form uniform and stable magnesium acetate
Liquid, the concentration of magnesium acetate solution are about 0.3mol/L;
Step 3. is using non-tight type combustion chamber as combustion chamber;
By magnesium acetate solution, continuously atomization sprays in the combustion chamber, and magnesium acetate solution is continuously atomized the flow of ejection in the combustion chamber
About 25mL/min;
Meanwhile it being passed through combustion-supporting gas in the combustion chamber, which is through the diluted oxygen of 25% nitrogen, and combustion-supporting gas is firing
Burning the indoor flow being passed through is about 50L/min;
To burn indoor substance successively-ignited, obtain burning powder;
Step 4. collects burning powder;
By the burning powder being collected into temperature condition roasted oreization about 3 hours of about 400 DEG C in Muffle furnace;
The good powder of mineralising in Muffle furnace is cooled to room temperature to get Mgo Nanopowder by step 5..
Embodiment 5
The present invention includes following process steps:
Step 1. dries magnesium acetate 3.5 hours under the conditions of about 100 DEG C of temperature, removes the crystallization water;
Acetic anhydride magnesium is dissolved in dehydrated alcohol by step 2., and the dissolving ratio of acetic anhydride magnesium and dehydrated alcohol is about
49.46:100;
In course of dissolution, glacial acetic acid is added into dehydrated alcohol, the additional amount of glacial acetic acid is about the magnesia amount of acetic anhydride
10%, solution rate and dissolution quality of the acetic anhydride magnesium in dehydrated alcohol are promoted with glacial acetic acid, form uniform and stable acetic acid
Magnesium solution, the concentration of magnesium acetate solution are saturation state (note: about 3.47mol/L);
Step 3. is using non-tight type combustion chamber as combustion chamber;
By magnesium acetate solution, continuously atomization sprays in the combustion chamber, and magnesium acetate solution is continuously atomized the flow of ejection in the combustion chamber
About 10mL/min;
Meanwhile it being passed through combustion-supporting gas in the combustion chamber, which is purity oxygen, the stream that combustion-supporting gas is passed through in the combustion chamber
Amount is about 15L/min;
To burn indoor substance successively-ignited, obtain burning powder;
Step 4. collects burning powder;
By the burning powder being collected into temperature condition roasted oreization about 2 hours of about 600 DEG C in Muffle furnace;
The good powder of mineralising in Muffle furnace is cooled to room temperature to get Mgo Nanopowder by step 5..
Embodiment 6
The present invention includes following process steps:
Step 1. dries magnesium acetate about 4 hours under the conditions of about 100 DEG C of temperature, removes the crystallization water;
Acetic anhydride magnesium is dissolved in dehydrated alcohol by step 2., and the dissolving ratio of acetic anhydride magnesium and dehydrated alcohol is about
28.4:100;
In course of dissolution, glacial acetic acid is added into dehydrated alcohol, the additional amount of glacial acetic acid is about the 9% of the magnesia amount of acetic anhydride,
Promote solution rate and dissolution quality of the acetic anhydride magnesium in dehydrated alcohol with glacial acetic acid, it is molten to form uniform and stable magnesium acetate
Liquid, the concentration of magnesium acetate solution are about 2mol/L;
Step 3. is using non-tight type combustion chamber as combustion chamber;
By magnesium acetate solution, continuously atomization sprays in the combustion chamber, and magnesium acetate solution is continuously atomized the flow of ejection in the combustion chamber
About 10mL/min;
Meanwhile it being passed through combustion-supporting gas in the combustion chamber, which is through the diluted oxygen of 25% nitrogen, and combustion-supporting gas is firing
Burning the indoor flow being passed through is about 20L/min;
To burn indoor substance successively-ignited, obtain burning powder;
Step 4. collects burning powder;
By the burning powder being collected into temperature condition roasted oreization about 3 hours of about 480 DEG C in Muffle furnace;
The good powder of mineralising in Muffle furnace is cooled to room temperature to get Mgo Nanopowder by step 5..
Embodiment 7
The present invention includes following process steps:
Step 1. dries magnesium acetate about 4.5 hours under the conditions of about 100 DEG C of temperature, removes the crystallization water;
Acetic anhydride magnesium is dissolved in dehydrated alcohol by step 2., and the dissolving ratio of acetic anhydride magnesium and dehydrated alcohol is about
2.84:100, forms uniform and stable magnesium acetate solution, and the concentration of magnesium acetate solution is about 0.2mol/L;
Step 3. is using non-tight type combustion chamber as combustion chamber;
By magnesium acetate solution, continuously atomization sprays in the combustion chamber, and magnesium acetate solution is continuously atomized the flow of ejection in the combustion chamber
About 25mL/min;
Meanwhile it being passed through combustion-supporting gas in the combustion chamber, which is through the diluted oxygen of 20% nitrogen, and combustion-supporting gas is firing
Burning the indoor flow being passed through is about 46.8L/min;
To burn indoor substance successively-ignited, obtain burning powder;
Step 4. collects burning powder;
By the burning powder being collected into temperature condition roasted oreization about 2.5 hours of about 530 DEG C in Muffle furnace;
The good powder of mineralising in Muffle furnace is cooled to room temperature to get Mgo Nanopowder by step 5..
Embodiment 8
The present invention includes following process steps:
Step 1. dries magnesium acetate about 5 hours under the conditions of about 100 DEG C of temperature, removes the crystallization water;
Acetic anhydride magnesium is dissolved in dehydrated alcohol by step 2., and the dissolving ratio of acetic anhydride magnesium and dehydrated alcohol is about
11.36:100;
In course of dissolution, glacial acetic acid is added into dehydrated alcohol, the additional amount of glacial acetic acid is about the 9% of the magnesia amount of acetic anhydride,
Promote solution rate and dissolution quality of the acetic anhydride magnesium in dehydrated alcohol with glacial acetic acid, it is molten to form uniform and stable magnesium acetate
Liquid, the concentration of magnesium acetate solution are about 0.8mol/L;
Step 3. is using non-tight type combustion chamber as combustion chamber;
By magnesium acetate solution, continuously atomization sprays in the combustion chamber, and magnesium acetate solution is continuously atomized the flow of ejection in the combustion chamber
About 20mL/min;
Meanwhile it being passed through combustion-supporting gas in the combustion chamber, which is purity oxygen, the stream that combustion-supporting gas is passed through in the combustion chamber
Amount is about 30L/min;
To burn indoor substance successively-ignited, obtain burning powder;
Step 4. collects burning powder;
By the burning powder being collected into temperature condition roasted oreization about 2 hours of about 660 DEG C in Muffle furnace;
The good powder of mineralising in Muffle furnace is cooled to room temperature to get Mgo Nanopowder by step 5..
The above various embodiments is only to illustrate the present invention, rather than its limitations.Although referring to the various embodiments described above to this hair
It is bright to be described in detail, those skilled in the art should understand that: the present invention still can be to the various embodiments described above
In specific technical solution modify perhaps equivalent replacement of some of the technical features and these modifications or replace
It changes, the spirit and scope of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (6)
1. a kind of Mgo Nanopowder preparation method, which is characterized in that the preparation method includes following process steps:
Step 1. dries magnesium acetate 3~5 hours under the conditions of 100 DEG C of temperature, removes the crystallization water;
Acetic anhydride magnesium is dissolved in dehydrated alcohol by step 2., and the dissolving ratio of acetic anhydride magnesium and dehydrated alcohol is 0.1~
50:100 forms uniform and stable magnesium acetate solution;
By magnesium acetate solution, continuously atomization sprays step 3. in the combustion chamber, while being passed through combustion-supporting gas in the combustion chamber;It will combustion
Indoor substance successively-ignited is burnt, burning powder is obtained;
Step 4. collects burning powder;
By the burning powder being collected into temperature condition roasted oreization 1~3 hour of 400~800 DEG C in Muffle furnace;
The good powder of mineralising in Muffle furnace is cooled to room temperature to get Mgo Nanopowder by step 5..
2. Mgo Nanopowder preparation method according to claim 1, which is characterized in that acetic anhydride described in step 2
In the course of dissolution in dehydrated alcohol glacial acetic acid is added in the dehydrated alcohol to promote acetic anhydride magnesium in anhydrous second in magnesium
Dissolution in alcohol, the additional amount of the glacial acetic acid are the 5~10% of the magnesia amount of acetic anhydride.
3. Mgo Nanopowder preparation method according to claim 1, which is characterized in that magnesium acetate described in step 2 is molten
The concentration of liquid is 0.01mol/L to saturated solution.
4. Mgo Nanopowder preparation method according to claim 1, which is characterized in that magnesium acetate described in step 3 is molten
The flow that liquid is continuously atomized ejection in the combustion chamber is 10~30mL/min;The flow that the combustion-supporting gas is passed through in the combustion chamber
For 15~50L/min.
5. according to claim 1 or the 4 Mgo Nanopowder preparation methods, which is characterized in that combustion-supporting gas described in step 3
Body is for purity oxygen or through the diluted oxygen of nitrogen.
6. according to claim 1 or the 4 Mgo Nanopowder preparation methods, which is characterized in that combustion chamber described in step 3
For non-tight type combustion chamber.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111714962A (en) * | 2019-03-21 | 2020-09-29 | 上海菲佐环保科技有限公司 | Preparation method of nano-filtration medium with adsorption capacity decomposition function |
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CN103265058A (en) * | 2013-05-20 | 2013-08-28 | 复旦大学 | Synthetic method of {111} crystal face preferred magnesium oxide material |
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2018
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CN102849760A (en) * | 2012-08-22 | 2013-01-02 | 中国科学院过程工程研究所 | Hollow nanometer magnesia microsphere and preparation method thereof |
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CN111714962A (en) * | 2019-03-21 | 2020-09-29 | 上海菲佐环保科技有限公司 | Preparation method of nano-filtration medium with adsorption capacity decomposition function |
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Application publication date: 20190201 |