CN106082287A - A kind of preparation method of magnesium oxide - Google Patents
A kind of preparation method of magnesium oxide Download PDFInfo
- Publication number
- CN106082287A CN106082287A CN201610420697.7A CN201610420697A CN106082287A CN 106082287 A CN106082287 A CN 106082287A CN 201610420697 A CN201610420697 A CN 201610420697A CN 106082287 A CN106082287 A CN 106082287A
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- magnesium oxide
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- magnesium
- precipitant
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention discloses the preparation method of a kind of magnesium oxide.Preparation process is as follows: solubility magnesium salt and precipitant are carried out liquid phase reactor, in course of reaction, the presoma of the magnesium oxide of three kinds of different-shapes can be prepared by the different types of surfactant of interpolation, interpolation solvent, reaction temperature and ul-trasonic irradiation time and power, after then carrying out the presoma of preparation filtering, wash, be dried and calcining, obtain the magnesium oxide of three kinds of different-shapes.The method is simple to operate, and applicable batch prepares the magnesium oxide of different-shape, and magnesium oxide material is with a wide range of applications at aspects such as catalysis, the energy and heat conduction.
Description
Technical field
Technical field of magnesium oxide of the present invention, specifically, relates to the preparation method of a kind of magnesium oxide.
Background technology
Magnesium oxide is the inorganic material of a kind of diverse in function, its heat conduction, ceramic industry, medical science, refractory material, optics and
The fields such as the energy all have broad application prospects.China is the country that magnesium resource enriches very much, and reasonably exploitation magnesium resource can push away
The dynamic national economic development.
Along with the development of science and technology, people find that physical property that inorganic material showed is generally and its shape under study for action
Looks have the biggest association, and therefore preparing the different pattern of material to study its performance has been the most natural science applied research
Focus.Pattern at the magnesium oxide reporting preparation has graininess, flower-shaped, lamellar, tubulose with bar-shaped etc., the preparation of every kind of pattern
Method is the most identical and purposes is all not quite similar.Zhu Yimin etc. (CN 201010246810.7, a kind of lamellar magnesium oxide
Preparation method) use ammonia to be prepared for the magnesium hydroxide presoma of lamellar in solubility magnesium salt as precipitant, through heating
Calcining has obtained flake nano magnesium oxide, and this magnesium oxide can be used as Infrared stealthy materials；Narottam Sutradhar etc.
(Sutradhar, N.et al.; Preparation of MgO nano-rods with strong catalytic
activity via hydrated basic magnesium carbonates. Mater Res Bull, 2011, 46,
It is 2163-2167.) that raw material adds the carbonic acid magnesium salt being prepared for being combined after coprecipitator with magnesium nitrate, is then prepared for after sintering
Nano bar-shape magnesium oxide, and this material as a kind of base catalyst can complete in 2 hours benzaldehyde 99% harmless
Catalysis.As can be seen here, the magnesium oxide preparing different-shape can expand its application at different aspect, how to efficiently control its shape
Looks will be the emphasis of research.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that one has controllability and prepares three kinds of different-shapes
(granular, bar-shaped and lamellar) method of magnesium oxide.
The technical solution used in the present invention is:
The present invention uses liquid phase method to be prepared for three kinds of different-shapes (granular, bar-shaped and lamellar) magnesium oxide presoma, then incites somebody to action
The magnesium oxide of three kinds of different-shapes (granular, bar-shaped and lamellar) is obtained after filtering, wash, be dried and calcining.Its preparation process is as follows:
Solubility magnesium salt and precipitant are carried out liquid phase reactor, prepares three kinds of not similar shapes by controlling dispersant, solvent and reaction condition
The presoma of the magnesium oxide of looks (granular, bar-shaped and lamellar), is filtered, is washed, dried, obtains through high-temperature calcination
Magnesium oxide to three kinds of different-shapes (granular, bar-shaped and lamellar).
In above-mentioned preparation method, the solubility magnesium salt of the magnesium oxide presoma of described three kinds of different-shapes of preparation is excellent
Select the one in magnesium nitrate, magnesium sulfate and magnesium chloride.
In above-mentioned preparation method, the preferred carbonic acid of precipitant of the magnesium oxide presoma of described three kinds of different-shapes of preparation
One in ammonium, carbamide, ammonium hydrogen carbonate and ammonium nitrate etc..
In above-mentioned preparation method, the dispersant that the magnesium oxide presoma of described three kinds of different-shapes of preparation needs is preferred
In sodium carboxymethyl cellulose, methylcellulose (methyl cellulose), polyvinyl alcohol or polyvinylpyrrolidone (PVP) one
Kind, addition is the 0.01 ~ 0.2% of solution quality.
In above-mentioned preparation method, the solvent that described preparation lamellar magnesium oxide presoma needs is ethanol solution, and it contains
Amount is the 5 ~ 50% of reaction solution.
In above-mentioned preparation method, the magnesium oxide presoma of described three kinds of different-shapes of preparation needs the reaction bar controlled
Part includes the conditions such as heating, ultrasound wave dispersion and mechanical agitation.
In above-mentioned preparation method, the reaction of the granular magnesium oxide presoma of described preparation is with above-mentioned soluble magnesium salt
One in (magnesium nitrate, magnesium sulfate or magnesium chloride) and in precipitant (ammonium carbonate, carbamide, ammonium hydrogen carbonate or ammonium nitrate etc.)
Kind, wherein Mg in solution2+Concentration and precipitant concentration ratio is for 1:5, and reaction reacts the most available at a temperature of 50 ~ 70 DEG C.
In above-mentioned preparation method, the reaction of the bar-shaped magnesium oxide presoma of described preparation is with above-mentioned soluble magnesium salt
One in (magnesium nitrate, magnesium sulfate or magnesium chloride) and in precipitant (ammonium carbonate, carbamide, ammonium hydrogen carbonate or ammonium nitrate)
Kind, the wherein magnesium ion (Mg in solution2+) concentration and precipitant concentration are than for 1:2 ~ 5, and add 0.01 ~ 0.1% mass ratio
Dispersant is (in sodium carboxymethylcellulose pyce, methylcellulose (methyl cellulose), polyvinyl alcohol or polyvinylpyrrolidone (PVP)
One), reaction at a temperature of 50 ~ 70 DEG C, react the most available.
In above-mentioned preparation method, the reaction of the lamellar magnesium oxide presoma of described preparation is with above-mentioned soluble magnesium salt
In a kind of precipitant (ammonium carbonate, carbamide, ammonium hydrogen carbonate or ammonium nitrate etc.) in one, wherein Mg in solution2+Concentration is with heavy
Shallow lake agent concentration is than for 1:1.5 ~ 6, and adds dispersant (sodium carboxymethylcellulose pyce, the methylcellulose of 0.01 ~ 0.15% mass ratio
One or more mixture in (methyl cellulose), polyvinyl alcohol or polyvinylpyrrolidone (PVP)), simultaneously molten
In liquid add ethanol (content be reaction solution volume 5 ~ 50%), reaction at a temperature of 50 ~ 70 DEG C, react the most available.
In above-mentioned preparation method, the calcining heat of the magnesium oxide of described three kinds of different-shapes of preparation is 500 ~ 700 DEG C,
The atmosphere furnace that stove is controllable temperature of used calcining or Muffle furnace.
Compared with prior art, there is advantages that and the invention discloses the preparation side of a kind of magnesium oxide
Method.The method can prepare the presoma of three kinds of different-shape magnesium oxide the most respectively by control condition, the most again by it
Carry out high-temperature calcination and obtain the magnesium oxide of three kinds of different-shapes.The method of the present invention is simple to operate, and applicable batch prepares not similar shape
The magnesium oxide of looks, and magnesium oxide material is with a wide range of applications at the aspect such as catalysis, the energy and heat conduction.
Accompanying drawing explanation
The SEM figure of Fig. 1 bar-shaped magnesium oxide presoma；
The SEM figure of the bar-shaped magnesium oxide of Fig. 2；
Fig. 3 bar-shaped magnesium oxide presoma and the XRD figure of magnesium oxide；
The SEM figure of Fig. 4 granular magnesium oxide presoma
The SEM figure of the granular magnesium oxide of Fig. 5；
The SEM figure of Fig. 6 lamellar magnesium oxide presoma；
The SEM figure of Fig. 7 lamellar magnesium oxide.
Detailed description of the invention
The present invention is explained further below in conjunction with specific embodiment, but invention is not done any type of limit by embodiment
Fixed.
Embodiment 1: be respectively configured the magnesium chloride hexahydrate (MgCl of 0.4mol/l2·6H2The ammonium carbonate of O) and 0.8 mol/l
((NH4)2CO3) solution, measure the MgCl of 0.4 mol/L (mol/L)2Solution 100 milliliters (ml) adds three hole flasks and is placed in
In water-bath, constant temperature is 60 DEG C and adds 0.2g polyvinylpyrrolidone (PVP).Again with the (NH of graduated cylinder amount 0.8 mol/l4)2CO3
Solution 100ml adds in constant pressure funnel, and constant speed drips in reaction vessel, then starts mechanical stirring device, controls its rotating speed and is
250 revs/min (rpm), the control response time is 10 minutes (min).Product is carried out vacuum filtration, 3 deionized waters
After washing and 1 ~ 2 washing with alcohol, it is then placed in the vacuum drying oven heat drying 12 hours (h) of 65 degrees Celsius (DEG C), obtains
The presoma of granular magnesium oxide.Magnesium oxide presoma is put in chamber type electric resistance furnace 650 DEG C, calcines 3h, after cooling down with furnace temperature just
Obtain granular magnesium oxide sample.Wherein Fig. 1 is bar-like the scanning electron microscope (SEM) photograph (SEM) of magnesium oxide presoma；Fig. 2 is bar-like oxidation
The SEM figure of magnesium；Fig. 3 is bar-like the X-ray diffractogram (XRD) of magnesium oxide and presoma.
Embodiment 2: be respectively configured 0.5 mol/L magnesium nitrate (Mg(NO3)2) and the ammonium hydrogen carbonate (NH of 1.2mol/l4HCO3)
Solution, measures the Mg(NO of 0.5 mol/L3)2It is 55 DEG C that solution 60 ml add three hole flasks to be placed in constant temperature in water-bath.Use again
The NH of graduated cylinder amount 1.2mol/l4HCO3Solution 60ml adds in constant pressure funnel, and constant speed drips in reaction vessel, then starts machinery
Agitating device, controlling its rotating speed is 300rpm, and the ultrasound wave simultaneously enabling 200 watts of (W) power is operated, whole reaction time
Between 15min.After product is carried out vacuum filtration, 3 deionized water wash and 1 ~ 2 washing with alcohol, it is then placed in 65 DEG C
Vacuum drying oven heat drying 12 hours, obtain the presoma of granular magnesium oxide.Magnesium oxide presoma is put into box resistance
In stove 600 DEG C, calcine 3h, after cooling down with furnace temperature, just obtain granular magnesium oxide sample.Fig. 4 is the SEM of granular magnesium oxide presoma
Figure, Fig. 5 is the SEM figure of granular magnesium oxide.
Embodiment 3: be respectively configured the magnesium sulfate (MgSO of 0.4 mol/L4) and the ammonium carbonate ((NH of 1.0 mol/l4)2CO3)
Solution, measures the MgSO of 0.4 mol/L4Solution 100 ml adds three hole flasks and is placed in constant temperature in water-bath and is 60 DEG C and adds
0.15g polyvinyl alcohol.Again with the (NH of graduated cylinder amount 1.0 mol/l4)2CO3Solution 100ml adds in constant pressure funnel, simultaneously at another
Adding the ethanol solution of 20 ml in the constant pressure funnel in individual hole, constant speed drips in reaction vessel, then starts mechanical stirring device,
Controlling its rotating speed is 250rpm, and the control response time is 25 min.Product is carried out vacuum filtration, 3 deionization washings
Wash with 1 ~ 2 washing with alcohol after, be then placed in the vacuum drying oven heat drying 12 hours of 65 DEG C, before obtaining granular magnesium oxide
Drive body.Magnesium oxide presoma is put in chamber type electric resistance furnace 650 DEG C, calcines 3h, after cooling down with furnace temperature, just obtain granular magnesium oxide
Sample.Fig. 6 is the SEM figure of lamellar magnesium oxide presoma, and Fig. 7 is the SEM figure of lamellar magnesium oxide.
Claims (10)
1. the preparation method of a magnesium oxide, it is characterised in that comprise the steps: solubility magnesium salt and precipitant are carried out liquid
Phase reaction, prepares the magnesium oxide presoma of three kinds of different-shapes, then by before it by controlling dispersant, solvent and reaction condition
Driving after body is dried washing, heating and calcining prepares granular, the bar-shaped or magnesium oxide of three kinds of different-shapes of lamellar.
Preparation method the most according to claim 1, it is characterised in that described solubility magnesium salt is magnesium nitrate, magnesium sulfate or chlorine
Change the one in magnesium.
Preparation method the most according to claim 1, it is characterised in that described precipitant is ammonium carbonate, carbamide, ammonium hydrogen carbonate
Or the one in ammonium nitrate.
Preparation method the most according to claim 1, it is characterised in that described dispersant is sodium carboxymethyl cellulose, methyl fibre
One in dimension element, polyvinyl alcohol or polyvinylpyrrolidone, addition is the 0.01 ~ 0.2% of solution quality.
Preparation method the most according to claim 1, it is characterised in that described solvent is ethanol solution, its content is molten for reaction
Liquid long-pending 5 ~ 50%.
Preparation method the most according to claim 1, it is characterised in that described reaction condition is heating, ultrasound wave disperses or machine
Tool stirs.
Preparation method the most according to claim 1, it is characterised in that the temperature of described calcining is 500 ~ 700 DEG C, described in forge
The atmosphere furnace that stove is controllable temperature burnt or Muffle furnace.
Preparation method the most according to claim 1, it is characterised in that the reaction of described granular magnesium oxide presoma is above
State solubility magnesium salt and precipitant, Mg2+Concentration and precipitant molar concentration rate are 1:5, and reaction is reacted at a temperature of 50 ~ 70 DEG C
Obtain.
Preparation method the most according to claim 1, it is characterised in that the reaction of described bar-shaped magnesium oxide presoma is above
State solubility magnesium salt and precipitant, Mg2+Concentration and precipitant concentration ratio for 1:2 ~ 5, and add 0.01 ~ 0.1% mass ratio point
Powder, reaction is reacted at a temperature of 50 ~ 70 DEG C and is obtained.
Preparation method the most according to claim 1, it is characterised in that the reaction of described lamellar magnesium oxide presoma is above
State solubility magnesium salt and precipitant, Mg2+Concentration and precipitant concentration are than for 1:1.5 ~ 6, and add 0.01 ~ 0.15% mass ratio
Dispersant, adds ethanol simultaneously in the solution, and ethanol content is the 5 ~ 50% of the volume of reaction solution, and reaction is at 50 ~ 70 DEG C
At a temperature of react and obtain.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107162026A (en) * | 2017-06-07 | 2017-09-15 | 常州西夏墅东方工具有限公司 | A kind of preparation method for nanometer magnesium oxide |
| CN107162025A (en) * | 2017-06-12 | 2017-09-15 | 镇江宇神动力能源有限公司 | A kind of preparation method of magnesia |
| CN107188207A (en) * | 2017-06-22 | 2017-09-22 | 山西大学 | A kind of preparation method for the magnesium oxide material that micron bar structure is assembled into by nanometer sheet |
| CN112167706A (en) * | 2020-09-28 | 2021-01-05 | 江苏中烟工业有限责任公司 | Additive for cigarette filter stick for reducing ammonia in cigarette smoke and application thereof |
| CN113072082A (en) * | 2021-03-31 | 2021-07-06 | 珠海格力新材料有限公司 | Preparation method and application of magnesium oxide flame retardant |
| CN113087207A (en) * | 2021-04-07 | 2021-07-09 | 山东理工大学 | Method for purifying non-ferrous metal beneficiation wastewater based on porous magnesium oxide cyclic preparation |
| CN113262753A (en) * | 2021-04-17 | 2021-08-17 | 北京化工大学 | Preparation method and application of millimeter-grade monodisperse magnesium oxide pellets |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107162026A (en) * | 2017-06-07 | 2017-09-15 | 常州西夏墅东方工具有限公司 | A kind of preparation method for nanometer magnesium oxide |
| CN107162025A (en) * | 2017-06-12 | 2017-09-15 | 镇江宇神动力能源有限公司 | A kind of preparation method of magnesia |
| CN107188207A (en) * | 2017-06-22 | 2017-09-22 | 山西大学 | A kind of preparation method for the magnesium oxide material that micron bar structure is assembled into by nanometer sheet |
| CN112167706A (en) * | 2020-09-28 | 2021-01-05 | 江苏中烟工业有限责任公司 | Additive for cigarette filter stick for reducing ammonia in cigarette smoke and application thereof |
| CN112167706B (en) * | 2020-09-28 | 2022-09-02 | 江苏中烟工业有限责任公司 | Additive for cigarette filter stick for reducing ammonia in cigarette smoke and preparation method and application thereof |
| CN113072082A (en) * | 2021-03-31 | 2021-07-06 | 珠海格力新材料有限公司 | Preparation method and application of magnesium oxide flame retardant |
| CN113087207A (en) * | 2021-04-07 | 2021-07-09 | 山东理工大学 | Method for purifying non-ferrous metal beneficiation wastewater based on porous magnesium oxide cyclic preparation |
| CN113262753A (en) * | 2021-04-17 | 2021-08-17 | 北京化工大学 | Preparation method and application of millimeter-grade monodisperse magnesium oxide pellets |
| CN113262753B (en) * | 2021-04-17 | 2023-08-04 | 北京化工大学 | Preparation method and application of millimeter-sized monodisperse magnesium oxide pellets |
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Application publication date: 20161109 |