CN107188207B - A kind of preparation method for the magnesium oxide material being assembled into micron bar structure by nanometer sheet - Google Patents
A kind of preparation method for the magnesium oxide material being assembled into micron bar structure by nanometer sheet Download PDFInfo
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- CN107188207B CN107188207B CN201710482622.6A CN201710482622A CN107188207B CN 107188207 B CN107188207 B CN 107188207B CN 201710482622 A CN201710482622 A CN 201710482622A CN 107188207 B CN107188207 B CN 107188207B
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- magnesium
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- nanometer sheet
- bar structure
- micron bar
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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
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The present invention relates to a kind of preparation method of magnesium oxide material for being assembled into micron bar structure by nanometer sheet, present invention aim to address the magnesia of existing preparation method of magnesia preparation there are specific surface areas small, poor activities, the inapparent technical problem of absorption property.The technical scheme is that a kind of preparation method for the magnesium oxide material for being assembled into micron bar structure by nanometer sheet, it is using seawater or salt lake bittern magnesium chloride as magnesium source, sodium carbonate is precipitating reagent, ethyl alcohol is as structure directing agent, presoma magnesium carbonate trihydrate is synthesized using low-temperature precipitation crystallisation, then calcining obtains the magnesia that micron bar structure is assembled by nanometer sheet in air.The present invention has strong operability, reproducible, non-environmental-pollution, the advantages such as can carry out at normal temperature, be easily industrialized；The micro- sodium rice material scatter of prepared magnesia is good, size uniformity and purity is high.
Description
Technical field
The invention belongs to field of inorganic material preparing technology, and in particular to a kind of oxidation that micron bar structure is assembled by nanometer sheet
The preparation method of magnesium material.
Background technique
With the rapid development of industrial or agricultural, increasing to the demand of heavy metal, toxic heavy metal is to drinking water quality
It pollutes also increasingly severe.Wherein the micro- pollution of heavy metal is always that huge obstinate type pollution is endangered in drinking water.Active carbon, work
The treatment effect of the conventional adsorbents pollutions micro- for heavy metal in drinking water such as property aluminium oxide, clay, zeolite is not significant.In recent years
Come, magnesia has been found to be one of high performance drinking water micro heavy ion removing medium, has low molten damage, high alkalinity
Excellent speciality, because O can be dissociateed2 -Ion and possess splendid antibiotic property, and due to isoelectric point up to 12.4 and to sun from
Son shows unique electrostatic capturing ability.
Magnesium is extracted from seawater or salt lake bittern, that is, is further processed and is closed as magnesium source using seawater or brine magnesium chloride
It is the new way that one kind high-qualityization utilizes magnesium resource at magnesia.Its advantage has raw material to be easy to get, low energy consumption, impurity is few, produced
Journey is convenient etc., and to the development and utilization important in inhibiting of China ocean and salt lake magnesium resource.It is mentioned from seawater or salt lake
The most popular method that magnesium prepares magnesia is precipitated crystal method.And the magnesia of existing precipitated crystal preparation is often micron order
It is solid rodlike, the disadvantages of there are specific surface areas small, poor activity, not significant absorption property.
Summary of the invention
Present invention aim to address the magnesia of existing preparation method of magnesia preparation, that there are specific surface areas is small, active
Difference, the inapparent technical problem of absorption property, provide a kind of system of magnesium oxide material that micron bar structure is assembled by nanometer sheet
Preparation Method.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: one kind being assembled into micron bar knot by nanometer sheet
The preparation method of the magnesium oxide material of structure, using seawater or salt lake bittern magnesium chloride as magnesium source, sodium carbonate is precipitating reagent, ethyl alcohol conduct
Structure directing agent synthesizes presoma magnesium carbonate trihydrate using low-temperature precipitation crystallisation, then calcining is obtained by nanometer in air
Piece is assembled into the magnesia of micron bar structure.
Further, a kind of preparation method for the magnesium oxide material being assembled into micron bar structure by nanometer sheet is specific to prepare
Steps are as follows:
1) pre-treatment in magnesium source: by seawater or brine, resulting crystalline mother solution is filtered to remove impurity, knot after shining halogen
Brilliant object obtains the purification brine of magnesium chloride containing；
2) precipitated crystal: adding water and ethyl alcohol to be configured to concentration in the purification brine for the magnesium chloride containing that step 1) obtains is 0.1
~3molL-1Magnesium chloride solution, configured magnesium chloride solution is added in the reactor tank of jacketed, to jacketed
It is passed through recirculated water in the collet of reactor tank, and its temperature is adjusted to 10~40 DEG C；Under agitation slowly into reactor tank
The molar concentration rate of addition and the isometric sodium carbonate liquor of magnesium chloride solution, the sodium carbonate liquor and magnesium chloride solution is 1:
1~1.2:1 after charging, continues stirring ageing, presoma magnesium carbonate trihydrate crystal is then obtained by filtration；
3) it roasts: the magnesium carbonate trihydrate crystal that step 2) obtains being washed 3~5 times with deionized water repeatedly and is placed on baking oven
In, it takes out, the magnesium carbonate trihydrate crystal after drying is placed in Muffle furnace, at 600~800 DEG C after dry 12h at 50 DEG C
Roasting temperature 2h is to get to the magnesia for being assembled into micron bar structure by nanometer sheet.
Further, the content of magnesium chloride is 3~4.5molL in the purification brine for the magnesium chloride containing that step 1) obtains-1。
Further, in step 2) when configuration magnesium chloride solution the additional amount of ethyl alcohol be magnesium chloride solution total volume 5~
30%.
Further, the revolving speed stirred in step 2) is 200~400rpm.
Further, the addition speed of sodium carbonate liquor is 0.4~1Lh in step 2)-1。
Further, the digestion time in step 2) is 2~4 hours.
Further, the nanometer sheet of the magnesium oxide material that micron bar structure is assembled by nanometer sheet with a thickness of 15~
20nm, micron bar length are 34~37 μm.
The beneficial effects of the present invention are:
1) present invention, by the way that ethyl alcohol is added as structure directing agent, regulates and controls presoma on the basis of existing precipitated crystal
The pattern of magnesium carbonate trihydrate, then through simple roasting to obtain the micron that, surface smooth nanometer sheet uniform by thickness assembles rodlike
Magnesia.
2) present invention has strong operability, reproducible, non-environmental-pollution, can carry out at normal temperature, be easily achieved work
The advantages such as industry；The micro- sodium rice material scatter of prepared magnesia is good, size uniformity and purity is high.Particularly, party's legal system
Standby magnesia has bright application prospect drinking the fields such as water sterilization and micro heavy ionic adsorption.
Detailed description of the invention
Fig. 1 is that 3500 times of low powers produced by the present invention for being assembled into micron bar structure magnesium oxide material by nanometer sheet scan electricity
Mirror figure；
Fig. 2 is that 25000 times of high powers produced by the present invention for being assembled into micron bar structure magnesium oxide material by nanometer sheet scan
Electron microscope.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples.
One of the present embodiment is assembled into the preparation method of the magnesium oxide material of micron bar structure by nanometer sheet, is with sea
Water or salt lake bittern magnesium chloride are magnesium source, and sodium carbonate is precipitating reagent, and ethyl alcohol is as structure directing agent, using low-temperature precipitation crystallisation
Synthesize presoma magnesium carbonate trihydrate, then calcining obtains the magnesia that micron bar structure is assembled by nanometer sheet in air.
Specific preparation process is as follows:
1) pre-treatment in magnesium source: by seawater or brine, resulting crystalline mother solution is filtered to remove impurity, knot after shining halogen
Brilliant object, obtaining content of magnesium chloride is 3~4.5molL-1Purification brine；
2) precipitated crystal: adding water and ethyl alcohol to be configured to concentration in the purification brine for the magnesium chloride containing that step 1) obtains is 0.1
~3molL-1Magnesium chloride solution, the additional amount of the ethyl alcohol is the 5~30% of magnesium chloride solution total volume；It will be configured
Magnesium chloride solution is added in the reactor tank of jacketed, recirculated water is passed through into the collet of the reactor tank of jacketed, and it is warm
Degree is adjusted to 10~40 DEG C；It is slowly added into reactor tank and chlorination in the case where speed of agitator is the stirring condition of 200~400rpm
The molar concentration rate of the isometric sodium carbonate liquor of magnesium solution, the sodium carbonate liquor and magnesium chloride solution is 1:1~1.2:1,
The addition speed of the sodium carbonate liquor is 0.4~1Lh-1；After charging, continue stirring 2~4 hours of ageing, then
Presoma magnesium carbonate trihydrate crystal is obtained by filtration；
3) it roasts: the magnesium carbonate trihydrate crystal that step 2) obtains being washed 3~5 times with deionized water repeatedly and is placed on baking oven
In, it takes out, the magnesium carbonate trihydrate crystal after drying is placed in Muffle furnace, at 600~800 DEG C after dry 12h at 50 DEG C
Roasting temperature 2h is described to be assembled into micron bar by nanometer sheet to get to the magnesia for being assembled into micron bar structure by nanometer sheet
The nanometer sheet of the magnesium oxide material of structure is 34~37 μm with a thickness of 15~20nm, micron bar length.
Embodiment 1
One of the present embodiment is assembled into the preparation method of the magnesium oxide material of micron bar structure by nanometer sheet, is with sea
Water or salt lake bittern magnesium chloride are magnesium source, and sodium carbonate is precipitating reagent, and ethyl alcohol is as structure directing agent, using low-temperature precipitation crystallisation
Synthesize presoma magnesium carbonate trihydrate, then calcining obtains the magnesia that micron bar structure is assembled by nanometer sheet in air.
Specific preparation process is as follows:
1) pre-treatment in magnesium source: by seawater or brine, resulting crystalline mother solution is filtered to remove impurity, knot after shining halogen
Brilliant object, obtaining content of magnesium chloride is 3molL-1Purification brine；
2) precipitated crystal: add water and ethyl alcohol to be configured to concentration in the purification brine for the magnesium chloride containing that step 1) obtains to be
1.5mol·L-1Magnesium chloride solution, the additional amount of the ethyl alcohol is the 5% of magnesium chloride solution total volume；By configured chlorination
Magnesium solution is added in the reactor tank of jacketed, is passed through recirculated water into the collet of the reactor tank of jacketed, and by its temperature tune
Section is 20 DEG C；It is slowly added in the case where speed of agitator is the stirring condition of 200rpm into reactor tank isometric with magnesium chloride solution
The molar concentration rate of sodium carbonate liquor, the sodium carbonate liquor and magnesium chloride solution is 1:1, the addition speed of the sodium carbonate liquor
Degree is 0.7Lh-1；After charging, continues stirring 3 hours of ageing, presoma magnesium carbonate trihydrate crystal is then obtained by filtration；
3) it roasts: the magnesium carbonate trihydrate crystal that step 2) obtains being washed 3~5 times with deionized water repeatedly and is placed on baking oven
In, taken out after dry 12h at 50 DEG C, the magnesium carbonate trihydrate crystal after drying be placed in Muffle furnace, 600 DEG C at a temperature of
2h is roasted to get to the magnesia for being assembled into micron bar structure by nanometer sheet.
Magnesium oxide material obtained is the length that the nanometer sheet for being about 15~20nm by thickness assembles in the present embodiment
For 34~37 μm of micron bar structures.
Embodiment 2
One of the present embodiment is assembled into the preparation method of the magnesium oxide material of micron bar structure by nanometer sheet, is with sea
Water or salt lake bittern magnesium chloride are magnesium source, and sodium carbonate is precipitating reagent, and ethyl alcohol is as structure directing agent, using low-temperature precipitation crystallisation
Synthesize presoma magnesium carbonate trihydrate, then calcining obtains the magnesia that micron bar structure is assembled by nanometer sheet in air.
Specific preparation process is as follows:
1) pre-treatment in magnesium source: by seawater or brine, resulting crystalline mother solution is filtered to remove impurity, knot after shining halogen
Brilliant object, obtaining content of magnesium chloride is 4molL-1Purification brine；
2) precipitated crystal: add water and ethyl alcohol to be configured to concentration in the purification brine for the magnesium chloride containing that step 1) obtains to be
0.1mol·L-1Magnesium chloride solution, the additional amount of the ethyl alcohol is the 15% of magnesium chloride solution total volume；By configured chlorine
Change magnesium solution to be added in the reactor tank of jacketed, be passed through recirculated water into the collet of the reactor tank of jacketed, and by its temperature
It is adjusted to 10 DEG C；It is slowly added in the case where speed of agitator is the stirring condition of 300rpm into reactor tank isometric with magnesium chloride solution
Sodium carbonate liquor, the molar concentration rate of the sodium carbonate liquor and magnesium chloride solution is 1.1:1, the sodium carbonate liquor plus
Entering speed is 0.4Lh-1；After charging, continues stirring 4 hours of ageing, presoma magnesium carbonate trihydrate is then obtained by filtration
Crystal；
3) it roasts: the magnesium carbonate trihydrate crystal that step 2) obtains being washed 3~5 times with deionized water repeatedly and is placed on baking oven
In, taken out after dry 12h at 50 DEG C, the magnesium carbonate trihydrate crystal after drying be placed in Muffle furnace, 700 DEG C at a temperature of
2h is roasted to get to the magnesia for being assembled into micron bar structure by nanometer sheet.
Magnesium oxide material obtained is the length that the nanometer sheet for being about 15~20nm by thickness assembles in the present embodiment
For 34~37 μm of micron bar structures.
Embodiment 3
One of the present embodiment is assembled into the preparation method of the magnesium oxide material of micron bar structure by nanometer sheet, is with sea
Water or salt lake bittern magnesium chloride are magnesium source, and sodium carbonate is precipitating reagent, and ethyl alcohol is as structure directing agent, using low-temperature precipitation crystallisation
Synthesize presoma magnesium carbonate trihydrate, then calcining obtains the magnesia that micron bar structure is assembled by nanometer sheet in air.
Specific preparation process is as follows:
1) pre-treatment in magnesium source: by seawater or brine, resulting crystalline mother solution is filtered to remove impurity, knot after shining halogen
Brilliant object, obtaining content of magnesium chloride is 4.5molL-1Purification brine；
2) precipitated crystal: add water and ethyl alcohol to be configured to concentration in the purification brine for the magnesium chloride containing that step 1) obtains to be
3mol·L-1Magnesium chloride solution, the additional amount of the ethyl alcohol is the 30% of magnesium chloride solution total volume；By configured chlorination
Magnesium solution is added in the reactor tank of jacketed, is passed through recirculated water into the collet of the reactor tank of jacketed, and by its temperature tune
Section is 40 DEG C；It is slowly added in the case where speed of agitator is the stirring condition of 400rpm into reactor tank isometric with magnesium chloride solution
The molar concentration rate of sodium carbonate liquor, the sodium carbonate liquor and magnesium chloride solution is 1.2:1, the addition of the sodium carbonate liquor
Speed is 1Lh-1；After charging, continues stirring 2 hours of ageing, presoma magnesium carbonate trihydrate crystal is then obtained by filtration；
3) it roasts: the magnesium carbonate trihydrate crystal that step 2) obtains being washed 3~5 times with deionized water repeatedly and is placed on baking oven
In, taken out after dry 12h at 50 DEG C, the magnesium carbonate trihydrate crystal after drying be placed in Muffle furnace, 800 DEG C at a temperature of
2h is roasted to get to the magnesia for being assembled into micron bar structure by nanometer sheet.
Magnesium oxide material obtained is the length that the nanometer sheet for being about 15~20nm by thickness assembles in the present embodiment
For 34~37 μm of micron bar structures.
Claims (7)
1. a kind of preparation method for the magnesium oxide material for being assembled into micron bar structure by nanometer sheet, with seawater or salt lake bittern chlorination
Magnesium is magnesium source, and sodium carbonate is precipitating reagent, and ethyl alcohol synthesizes three water of presoma as structure directing agent, using low-temperature precipitation crystallisation
Magnesium carbonate, then calcining obtains the magnesia that micron bar structure is assembled by nanometer sheet in air；It is characterized in that, specific preparation
Steps are as follows:
1) pre-treatment in magnesium source: by seawater or brine, resulting crystalline mother solution is filtered to remove impurity, crystal after shining halogen,
Obtain the purification brine of magnesium chloride containing；
2) precipitated crystal: by the purification brine for the magnesium chloride containing that step 1) obtains add water and ethyl alcohol be configured to concentration be 0.1~
3mol·L-1Magnesium chloride solution, configured magnesium chloride solution is added in the reactor tank of jacketed, to the anti-of jacketed
It answers and is passed through recirculated water in the collet of tank, and its temperature is adjusted to 10~40 DEG C；Slowly add into reactor tank under agitation
Enter the sodium carbonate liquor isometric with magnesium chloride solution, the molar concentration rate of the sodium carbonate liquor and magnesium chloride solution is 1:1
~1.2:1 after charging, continues stirring ageing, presoma magnesium carbonate trihydrate crystal is then obtained by filtration；
3) it roasts: the magnesium carbonate trihydrate crystal that step 2) obtains being washed 3~5 times with deionized water repeatedly and is placed in baking oven,
It takes out, the magnesium carbonate trihydrate crystal after drying is placed in Muffle furnace, in 600~800 DEG C of temperature after dry 12h at 50 DEG C
Lower roasting 2h is to get to the magnesia for being assembled into micron bar structure by nanometer sheet.
2. a kind of preparation method of magnesium oxide material that micron bar structure is assembled by nanometer sheet according to claim 1,
It is characterized by: the content of magnesium chloride is 3~4.5molL in the purification brine for the magnesium chloride containing that step 1) obtains-1。
3. a kind of preparation method of magnesium oxide material that micron bar structure is assembled by nanometer sheet according to claim 1,
It is characterized by: the additional amount of ethyl alcohol is the 5~30% of magnesium chloride solution total volume when configuration magnesium chloride solution in step 2).
4. a kind of preparation method of magnesium oxide material that micron bar structure is assembled by nanometer sheet according to claim 1,
It is characterized by: the revolving speed stirred in step 2) is 200~400rpm.
5. a kind of preparation method of magnesium oxide material that micron bar structure is assembled by nanometer sheet according to claim 1,
It is characterized by: the addition speed of sodium carbonate liquor is 0.4~1Lh in step 2)-1。
6. a kind of preparation method of magnesium oxide material that micron bar structure is assembled by nanometer sheet according to claim 1,
It is characterized by: the digestion time in step 2) is 2~4 hours.
7. a kind of preparation method of magnesium oxide material that micron bar structure is assembled by nanometer sheet according to claim 1,
It is characterized by: be assembled into step 3) by nanometer sheet the nanometer sheet of the magnesium oxide material of micron bar structure with a thickness of 15~
20nm, micron bar length are 34~37 μm.
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| CN109437256B (en) * | 2018-11-13 | 2021-05-14 | 武汉纺织大学 | Micro-nano magnesium oxide flame retardant and preparation method thereof |
| CN113209959B (en) * | 2021-05-12 | 2023-01-24 | 昆明理工大学 | Preparation method of load type rod-shaped magnesium oxide composite antibacterial agent |
| KR20240044446A (en) | 2021-08-09 | 2024-04-04 | 조인트 스탁 컴퍼니 카우스티크 | High purity magnesium oxide and method for producing the same |
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| CN106082287A (en) * | 2016-06-14 | 2016-11-09 | 中山大学 | A kind of preparation method of magnesium oxide |
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Effective date of registration: 20200508 Address after: 046200 Fuyang circular economy industrial zone, Changzhi, Shanxi, Xiangyuan Patentee after: SHANXI MOUNTAIN POWER PLATINUM CAROLINA RUBBER BELT Co.,Ltd. Address before: 030006 Taiyuan City, Shanxi province city road, No. 92 Patentee before: Shanxi University |