CN107285347A - A kind of method that utilization magnesite prepares porous spherical basic carbonate magnesium crystal - Google Patents
A kind of method that utilization magnesite prepares porous spherical basic carbonate magnesium crystal Download PDFInfo
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- CN107285347A CN107285347A CN201710706009.8A CN201710706009A CN107285347A CN 107285347 A CN107285347 A CN 107285347A CN 201710706009 A CN201710706009 A CN 201710706009A CN 107285347 A CN107285347 A CN 107285347A
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- C—CHEMISTRY; METALLURGY
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/24—Magnesium carbonates
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- 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
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- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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Abstract
A kind of method that utilization magnesite prepares porous spherical basic carbonate magnesium crystal, belongs to mineral manufacture field.The preparation method includes calcined magnesite, obtains active oxidation magnesium dust；Digestion prepares Mg (OH)2Suspension；It is passed through CO2Prepare precursor aqueous solution Mg (HCO3)2；To precursor aqueous solution Mg (HCO3)2Middle addition NaOH solution, adjusts pH value, to Mg (HCO3)2Lauryl sodium sulfate is added in solution, crystallizes, be incubated, filter, wash, dry, that is, obtain porous spherical basic carbonate magnesium crystal.Magnesite calcining is obtained extra light calcined magnesia by this method water chestnut using magnesium ore deposit as raw material, using lauryl sodium sulfate as crystal control agent, prepares porous spherical basic carbonate magnesium crystal using hydration method at ambient pressure.The product morphology prepared is porous spherical, purity is high, crystal formation is complete, pattern is uniform.
Description
Technical field
The invention belongs to mineral manufacture field, and in particular to it is brilliant that one kind prepares porous spherical basic magnesium carbonate using magnesite
The method of body.
Background technology
Basic magnesium carbonate (4MgCO3·Mg(OH)2·4H2O it is) a kind of important inorganic mineral powder material, because with good
Fillibility well, mobility, dispersiveness, and interfacial property is excellent, intensity is high, high temperature resistant, fire-retardant fireproof suppression cigarette, nontoxic, matter
Gently, the performance characteristics such as loose, are widely used in the various necks such as rubber, coating, chemical industry, medicine, machinery, metallurgy, building, environmental protection
Domain, thus it is of great interest at home and abroad.
Due to being restricted by production technology and technical costs, large-scale production is not yet realized in the preparation of basic magnesium carbonate, because
And the low cost feedstock and technique for seeking suitable large-scale industrial production are extremely urgent.
Common basic carbonate magnesium crystal preparation method has two kinds.One kind is with MgCl2·6H2O、Mg(NO3)2·6H2O、
MgSO4·7H2The soluble magnesium salts such as O and Na2CO3、NaHCO3、NH4HCO3、(NH4)2CO3It is raw material Direct precipitation Deng carbonate
Method, is mixed by the way of another raw material using a kind of raw material is instilled, obtains different-shape basic carbonate magnesium crystal；The method due to
Speed is slow, can produce brine waste, prepare cost height, it is difficult to realize industrialized production, extensive use is restricted.It is another to be
Using natural minerals such as dolomite, magnesite, shepardites as raw material, basic magnesium carbonate is prepared using hydration method.With direct precipitation method
Compare, this method raw material is cheap and easy to get, preparation condition is gentle, and cost is greatly lowered, and is easier to realize industrialized production.
China's magnesite resource is abundant and superior in quality, wherein, 35.16 hundred million tons of resource reserve is found out in Liaoning, accounts for the whole nation
The 86.39% of magnesite gross reserves, is one of extraordinary mineral resources of Liaoning Province's advantage.Past due to adopt richness abandon it is poor, disorderly adopt and rob a mine,
So that high-quality mineral resources are drastically reduced, and a large amount of low-grade magnesites go out of use and take up an area stacking, cause resource significant wastage.
Mineral resources are the resources of the non-renewable advantage of China, how to realize that to its efficient utilizes be an important subject.With
Magnisite is raw material, studies the preparation method of basic magnesium carbonate, to reduction product cost, efficient high-value-use mineral resources
Have important practical significance.
This invention uses magnesite for raw material, and efficiently using reserves than more rich high-quality magnesite mineral, its is main
Composition is magnesium carbonate (MgCO3), porous spherical basic carbonate magnesium crystal is prepared using reasonable process.By the experimental study of system
And optimization design, finally invent that technique is simple, cost is low, prepared by the uniform porous spherical basic carbonate magnesium crystal of appearance and size
Method.With a process for preparing porous spherical basic magnesium carbonate crystal purity is high, whiteness is good and microballoon average diameter for 4.0~
10.0μm。
The content of the invention
The purpose of the present invention is in view of the deficienciess of the prior art, provide one kind prepares porous spherical alkali using magnesite
The method of formula carbonic acid magnesium crystal.Magnesite calcining is obtained extra light calcined magnesia, with dodecane by this method using magnesite as raw material
Base sodium sulphate is crystal control agent, prepares porous spherical basic carbonate magnesium crystal using hydration method at ambient pressure.By repeatedly examination
Test, finally invented the preparation method of porous spherical basic magnesium carbonate, with a process for preparing product purity is high, crystal formation is complete
Whole, pattern is uniform, and its structure is different from the light magnesium carbonate in existing report.
To achieve the above object and use technical scheme be：
A kind of method that utilization magnesite prepares porous spherical basic carbonate magnesium crystal, comprises the steps：
(1) calcined magnesite
Magnesite is calcined, makes magnesite resolution ratio >=98%, obtains activated magnesia, using citric acid method to it
It is active to be detected, Coloring Time≤30s；
Activated magnesia is crushed, the active oxidation magnesium dust of granularity≤- 74 μm is obtained；
(2) digestion prepares Mg (OH)2Suspension
Active oxidation magnesium dust to obtain adds deionized water, is sufficiently stirred for being configured to the initial slurries of MgO as raw material；
Wherein, in mass ratio, active oxidation magnesium dust：Deionized water=1：(12~50)；
The initial slurries of MgO are stirred into 1.0~5.0h at 55~65 DEG C, room temperature is air-cooled to, Mg (OH) is made2Suspension；
(3) precursor aqueous solution Mg (HCO are prepared3)2
Under the conditions of 0~10 DEG C, to Mg (OH)2CO is passed through in suspension2Gas, is stirred simultaneously, when solution ph is
When 7.0~7.5, stop ventilation and stir, filtered, obtain transparent clarification precursor aqueous solution Mg (HCO3)2；
Wherein, it is passed through CO2The Ventilation Rate of gas is 0.10~0.16m3/h；
(4) precursor aqueous solution Mg (HCO3)2Pyrolysis
To precursor aqueous solution Mg (HCO3)2Middle addition NaOH solution, adjusts pH value, obtains the Mg that pH value is 8.0~10.5
(HCO3)2Solution；
By the Mg (HCO that pH value is 8.0~10.53)2Solution is placed in crystallizer, with 1 DEG C/min~5 DEG C/min heating
Speed is heated up, meanwhile, it is stirred with 100~500r/min stir speed (S.S.), when mould temperature reaches 60~80 DEG C
When, to Mg (HCO3)2Lauryl sodium sulfate is added in solution, wherein, lauryl sodium sulfate addition is Mg (HCO3)2It is molten
The 1 ‰ of liquid mass fraction~5 ‰；
After addition is finished, then constant temperature 30~120min of insulation stops heating and stirs, filter, wash, dry, produce
To porous spherical basic carbonate magnesium crystal.
In described step (1), described calcining, calcining heat is 600~800 DEG C, and calcination time is 1.0~3.0h.
In described step (2), the temperature of described deionized water is 70~100 DEG C.
In described step (3), described stirring, its stir speed (S.S.) is 200~500r/min.
In described step (4), the molar concentration of described NaOH solution is 0.5~2.0mol/L.
Porous spherical basic carbonate magnesium crystal prepared by the present invention, its molecular formula is 4MgCO3·Mg(OH)2·4H2O, its
Pattern is porous spherical, and the average diameter of porous ball is 4.0~10.0 μm.Porous ball surface is to be accumulated in layer by nanometer sheet
" rose " structure, because between nanometer sheet exist cavity form loose structure.
Above-mentioned technical proposal is further illustrated：
During implementation this invention prepares porous spherical basic carbonate magnesium crystal, the main ginseng of product quality is influenceed
Number includes the resolution ratio and MgO activity, solid-to-liquid ratio, CO of magnesite2Flow velocity, it is passed through CO2When temperature, reaction temperature, reaction when
Between, Mg (HCO3)2The factors such as solution ph, lauryl sodium sulfate consumption, mixing speed.
(1) resolution ratio of magnesite and MgO activity.Resolution ratio and the MgO activity of magnesite are to basic carbonate magnesium crystal
Formation has critical influence, (changes colour wherein calcining obtained activated magnesia when choosing magnesite resolution ratio >=98%
Time≤30s) the basic carbonate magnesium crystal prepared is more satisfactory.
(2) solid-to-liquid ratio.MgO and H2Mg (HCO in O mass ratio influence reaction system3)2Solution degree of supersaturation, low supersaturation
Degree is conducive to nucleus growth, crystal nucleation rate relative reduction, and high degree of supersaturation is conducive to crystal nucleation, growth rate reduction.
In order that crystal morphology reaches most preferably, the mass ratio for the MgO/ water that the present invention is used is 1/50~1/12.
(3)CO2Flow velocity and be passed through CO2When temperature.CO2Mg (HCO in flow rate effect reaction system3)2Solution Mg2+It is molten
Extracting rate and degree of supersaturation, Mg2+Dissolution rate is high, and products collection efficiency is high；Low degree of supersaturation is conducive to nucleus growth, crystal nucleation rate
Relative reduction, high degree of supersaturation is conducive to crystal nucleation, growth rate reduction, in order to obtain the alkali of preferable pattern and higher yields
Formula carbonic acid magnesium crystal, it is of the invention by CO2Flow control is in 0.10m3/ h~0.16m3/h。
It is passed through CO2When, temperature influence Mg2+The existence of ion in the solution, when temperature is more than 10 DEG C, has been generated
Mg(HCO3)2Solution can be pyrolyzed generation MgCO3·5H2O、MgCO3·3H2O、4MgCO3·Mg(OH)2·5H2The hydrocarbonate of magnesias such as O
Precipitation, will so cause Mg in solution2+Concentration is reduced, the yield of final influence product, therefore, temperature control of the present invention 0~
10℃。
(4) reaction temperature.In pyrolysis Mg (HCO3)2Solution is prepared in porous spherical basic magnesium carbonate crystallization process, reaction temperature
Degree should be strict controlled in certain limit, the too low easy generation magnesium carbonate trihydrate of temperature, and is unfavorable for the formation of basic magnesium carbonate, temperature
The scattered and sponginess of high influence basic magnesium carbonate is spent, while also result in the waste of the energy.Reaction temperature exists in the present invention
The basic magnesium carbonate crystal morphology obtained at 60~80 DEG C is more satisfactory, is porous spherical, uniform particle sizes, microballoon average diameter
For 4.0~10.0 μm.
(5) reaction time.There is direct influence in reaction time to synthesis product morphology and thing phase composition, and the reaction time is not
Can be too short, the formation of basic magnesium carbonate needs the adequate reaction time, but the uniformity of reaction time long product morphology has dropped
Low, agglomeration is obvious.At 65~85 DEG C, when reacted between be 45~85min when, crystal morphology is more satisfactory, uniform particle sizes,
For porous spherical, microballoon average diameter is 4.0~10.0 μm.Utilize the wire side spacing d values and JCPDS 00- at X-ray diffraction peak
025-0513 4MgCO3·Mg(OH)2·4H2The d values of O standard cards are corresponded, and peak shape is sharp, and free from admixture peak is present,
Illustrate the 414 type porous spherical basic carbonate magnesium crystals of all well-crystallizeds of reaction product.
(6)Mg(HCO3)2Solution ph.Mg(HCO3)2Solution ph has a direct impact to the pattern of synthetic product, pH value
It is too low, form porous rhabdolith；PH value is too high, then forms random flower-like crystallite, and pH value is controlled at 8.0~10.5, brilliant
Bodily form looks are more satisfactory, are porous spherical, and microspherulite diameter is uniform, and average diameter is 4.0~10.0 μm.
(7) lauryl sodium sulfate consumption.The addition of auxiliary agent plays key to the pattern and composition of basic carbonate magnesium crystal
Effect.By adding the non-crystalline substance for growing crystal face in crystal control agent, control nucleus nucleation and growth process in preparation process
Face energy, makes its oriented growth.Using lauryl sodium sulfate as crystal control agent, addition is that forerunner is molten in preparation process
Liquid Mg (HCO3)2The 1 ‰ of quality~5 ‰ (wt), prepared porous spherical basic carbonate magnesium crystal average diameter for 4.0~
10.0 μm, uniform particle sizes, pattern is preferable.
(8) mixing speed.In order that precursor aqueous solution even concentration, temperature are consistent in pyrolytic process, in crystallizer
Precursor aqueous solution will be stirred all the time, and mixing speed should be controlled within the specific limits.When mixing speed is 100~500r/min
When, comparatively ideal porous spherical basic carbonate magnesium crystal can be prepared.
The method that a kind of utilization magnesite of the present invention prepares porous spherical basic carbonate magnesium crystal, alkali is prepared with existing
The technical method of formula carbonic acid magnesium crystal is compared, and this invention has the following advantages that：
(1) raw material sources are extensive.China is one of high-quality magnesite ore reserves most abundant country, using it as raw material, can be shown
Write the preparation cost of reduction basic carbonate magnesium crystal.
(2) technique is simple.Whole technical process is divided into four big processes, and each process needs the relevant parameter controlled to compare
It is less, it is simple to operate.
(3) production equipment is relatively simple.Roaster, crystallizer and drying equipment are the three main bodies in whole preparation technology
Equipment, remaining is large-scale skewed slot, mixing and mixing plant etc. of acid and alkali-resistance, therefore small investment, easy industrialization, and main equipment
Easily realize and automatically control.
(4) in porous spherical basic carbonate magnesium crystal preparation process, grown using additive control high preferred orientation, so that
Control pattern.
(5) the porous spherical basic magnesium carbonate produced using this method is filled the domestic gaps, and doses rubber, plastics contour
Both the consumption of rubber, plastics can be reduced in Molecularly Imprinted Polymer, goods cost is reduced, the fire-retardant and machinery of material is remarkably improved again
Mechanical property, reduces the probability of happening of fire incident, is that society reduces unnecessary loss, improves people's sense of security and life matter
Amount, realizes environment-friendly flame retardant.
Brief description of the drawings
Fig. 1 is process flow diagram of the invention.
Fig. 2 is the SEM figures of porous spherical basic carbonate magnesium crystal prepared by the embodiment of the present invention 1；(multiplication factor 200 ×)
Fig. 3 is the SEM figures of porous spherical basic carbonate magnesium crystal prepared by the embodiment of the present invention 1；(multiplication factor 4500
×)
Fig. 4 is the X ray diffracting spectrum of porous spherical basic carbonate magnesium crystal prepared by the embodiment of the present invention 1.
Embodiment
With reference to embodiment, the present invention is described in further detail.
In following examples, the magnesite produced using Liaoning is raw material, prepares porous spherical basic carbonate magnesium crystal.
In following examples, thermal decomposition product pattern is observed using JEOL companies JSM-6360LV types SEM,
The diameter of porous bar-shaped product is measured by SEM map analysis；The thing phase of thermal decomposition product is detected using X-Pert types x-ray diffractometer
Composition.
Embodiment 1
A kind of method that utilization magnesite prepares porous spherical basic carbonate magnesium crystal, its process flow diagram is shown in Fig. 1, tool
Body comprises the steps：
(1) calcined magnesite
Magnesite is subjected to calcining 3.0h at a temperature of 750 DEG C, makes magnesite resolution ratio up to 99%, obtains active oxidation
Magnesium, detects that Coloring Time is 30s using citric acid method to its activity；
Activated magnesia is carried out to be crushed to -74 μm, active oxidation magnesium dust is obtained；
(2) digestion prepares Mg (OH)2Suspension
Using obtained active oxidation magnesium dust as raw material, 90 DEG C of deionized water is added, is sufficiently stirred for being configured to MgO initial
Slurry；Wherein, in mass ratio, active oxidation magnesium dust：Deionized water=1：40；
The initial slurries of MgO are placed in 60 DEG C of thermostat water baths, 3.5h is stirred, is air-cooled to room temperature, Mg (OH) is made2Suspend
Liquid；
(3) precursor aqueous solution Mg (HCO are prepared3)2
By Mg (OH)2Suspension is placed in 5 DEG C of water-baths, with 0.14m3/ h Ventilation Rate is to Mg (OH)2Lead in suspension
Enter CO2Gas, while be stirred with 500r/min stir speed (S.S.), when solution ph is 7.0~7.5, stop ventilation and
Stirring, is filtered, obtains transparent clarification precursor aqueous solution Mg (HCO3)2；
(4) precursor aqueous solution Mg (HCO3)2Pyrolysis
To precursor aqueous solution Mg (HCO3)2Middle addition molar concentration is 1.0mol/LNaOH solution, adjusts pH value, obtains pH value
For 9.0 Mg (HCO3)2Solution；
By the Mg (HCO that pH value is 9.03)2Solution is placed in crystallizer, is heated up with 1 DEG C/min heating rate, together
When, it is stirred with 500r/min stir speed (S.S.), when mould temperature reaches 80 DEG C, to Mg (HCO3)2Ten are added in solution
Sodium dialkyl sulfate, wherein, lauryl sodium sulfate addition is Mg (HCO3)2The 3 ‰ of liquid quality fraction；
After addition is finished, constant temperature is incubated 60min, then stops heating and stirs, and filters, washs, dries, that is, obtains porous
Spherical basic carbonate magnesium crystal, its molecular formula is 4MgCO3·Mg(OH)2·4H2O。
Porous spherical basic carbonate magnesium crystal manufactured in the present embodiment is tested and analyzed, its SEM figure is shown in Fig. 2, from Fig. 2
It can be seen that, the basic magnesium carbonate crystal morphology of preparation is porous spherical, and the average diameter of porous ball is 10.0 μm.Porous ball surface is
" rose " structure (see Fig. 3) accumulated in layer by nanometer sheet, forms porous because there is cavity between nanometer sheet
Structure.
The X ray diffracting spectrum of the porous spherical basic carbonate magnesium crystal of preparation is shown in Fig. 4, its diffraction maximum and JCPDS 00-
025-0513 basic magnesium carbonates (4MgCO3·Mg(OH)2·4H2O XRD standard diagrams) are consistent, and lattice constant isβ=114.44 °, peak shape is sharp, and free from admixture peak is present.Measurement results show
Thermal decomposition product is porous spherical basic carbonate magnesium crystal, uniform particle sizes, complete crystallization.
Embodiment 2
A kind of method that utilization magnesite prepares porous spherical basic carbonate magnesium crystal, comprises the steps：
(1) calcined magnesite
Magnesite is subjected to calcining 3.0h at a temperature of 700 DEG C, it is 98% to make magnesite resolution ratio, obtains active oxidation
Magnesium, detects that Coloring Time is 28s using citric acid method to its activity；
Activated magnesia is carried out to be crushed to the active oxidation magnesium dust that granularity is -72 μm；
(2) digestion prepares Mg (OH)2Suspension
Using obtained active oxidation magnesium dust as raw material, 70 DEG C of deionized water is added, is sufficiently stirred for being configured to MgO initial
Slurry；Wherein, in mass ratio, active oxidation magnesium dust：Deionized water=1：50；
The initial slurries of MgO are placed in 55 DEG C of thermostat water baths, 5.0h is stirred, is air-cooled to room temperature, Mg (OH) is made2Suspend
Liquid；
(3) precursor aqueous solution Mg (HCO are prepared3)2
By Mg (OH)2Suspension is placed under 0 DEG C of water-bath, using Ventilation Rate as 0.10m3/ h, to Mg (OH)2In suspension
It is passed through CO2Gas, while being stirred with 300r/min stir speed (S.S.), when solution ph is 7.0~7.5, stops ventilation
And stirring, filtered, obtain transparent clarification precursor aqueous solution Mg (HCO3)2；
(4) precursor aqueous solution Mg (HCO3)2Pyrolysis
To precursor aqueous solution Mg (HCO3)2Middle addition molar concentration is 0.5mol/LNaOH solution, adjusts pH value, obtains pH value
For 8.0 Mg (HCO3)2Solution；
By the Mg (HCO that pH value is 8.03)2Solution is placed in crystallizer, is heated up with 5 DEG C/min heating rate, together
When, it is stirred with 100r/min stir speed (S.S.), when mould temperature reaches 70 DEG C, to Mg (HCO3)2Ten are added in solution
Sodium dialkyl sulfate, wherein, lauryl sodium sulfate addition is Mg (HCO3)2The 1 ‰ of liquid quality fraction；
After addition is finished, constant temperature is incubated 30min, then stops heating and stirs, and filters, washs, dries, that is, obtains alkali formula
Carbonic acid magnesium crystal, its molecular formula is 4MgCO3·Mg(OH)2·4H2O, pattern is porous spherical, and the average diameter of porous ball is
5.0μm。
Embodiment 3
A kind of method that utilization magnesite prepares porous spherical basic carbonate magnesium crystal, comprises the steps：
(1) calcined magnesite
Magnesite is subjected to calcining 1.0h at a temperature of 800 DEG C, it is 99% to make magnesite resolution ratio, obtains active oxidation
Magnesium, detects that Coloring Time is 30s using citric acid method to its activity；
Activated magnesia is carried out to be crushed to the active oxidation magnesium dust that granularity is -70 μm；
(2) digestion prepares Mg (OH)2Suspension
Active oxidation magnesium dust to obtain adds 100 DEG C of deionized water, is sufficiently stirred at the beginning of being configured to MgO as raw material
Expect slurry；Wherein, in mass ratio, active oxidation magnesium dust：Deionized water=1：12；
The initial slurries of MgO are placed in 65 DEG C of thermostat water baths, 1.0h is stirred, is air-cooled to room temperature, Mg (OH) is made2Suspend
Liquid；
(3) precursor aqueous solution Mg (HCO are prepared3)2
By Mg (OH)2Suspension is placed in 10 DEG C of water-baths, using Ventilation Rate as 0.16m3/ h is to Mg (OH)2In suspension
It is passed through CO2Gas, while being stirred with 200r/min stir speed (S.S.), when solution ph is 7.0~7.5, stops ventilation
And stirring, filtered, obtain transparent clarification precursor aqueous solution Mg (HCO3)2；
(4) precursor aqueous solution Mg (HCO3)2Pyrolysis
To precursor aqueous solution Mg (HCO3)2Middle addition molar concentration is 2.0mol/LNaOH solution, adjusts pH value, obtains pH value
For 10.5 Mg (HCO3)2Solution；
By the Mg (HCO that pH value is 10.53)2Solution is placed in crystallizer, is heated up with 1 DEG C/min heating rate, together
When, it is stirred with 400r/min stir speed (S.S.), when mould temperature reaches 60 DEG C, to Mg (HCO3)2Ten are added in solution
Sodium dialkyl sulfate, wherein, lauryl sodium sulfate addition is Mg (HCO3)2The 5 ‰ of liquid quality fraction；
After addition is finished, constant temperature is incubated 120min, then stops heating and stirs, and filters, washs, dries, that is, obtains alkali
Formula carbonic acid magnesium crystal, its molecular formula is 4MgCO3·Mg(OH)2·4H2O, pattern is porous spherical, and the average diameter of porous ball is
4.0μm。
Claims (6)
1. a kind of method that utilization magnesite prepares porous spherical basic carbonate magnesium crystal, it is characterised in that comprise the steps：
(1) calcined magnesite
Magnesite is calcined, makes magnesite resolution ratio >=98%, obtains activated magnesia, using citric acid method to its activity
Detected, Coloring Time≤30s；
Activated magnesia is crushed, the active oxidation magnesium dust of granularity≤- 74 μm is obtained；
(2) digestion prepares Mg (OH)2Suspension
Active oxidation magnesium dust to obtain adds deionized water, is sufficiently stirred for being configured to the initial slurries of MgO as raw material；Wherein,
In mass ratio, active oxidation magnesium dust：Deionized water=1：(12~50)；
The initial slurries of MgO are stirred into 1.0~5.0h at 55~65 DEG C, room temperature is air-cooled to, Mg (OH) is made2Suspension；
(3) precursor aqueous solution Mg (HCO are prepared3)2
Under the conditions of 0~10 DEG C, to Mg (OH)2CO is passed through in suspension2Gas, is stirred simultaneously, when solution ph is 7.0
When~7.5, stop ventilation and stir, filtered, obtain transparent clarification precursor aqueous solution Mg (HCO3)2；
Wherein, it is passed through CO2The Ventilation Rate of gas is 0.10~0.16m3/h；
(4) precursor aqueous solution Mg (HCO3)2Pyrolysis
To precursor aqueous solution Mg (HCO3)2Middle addition NaOH solution, adjusts pH value, obtains the Mg (HCO that pH value is 8.0~10.53)2It is molten
Liquid；
By the Mg (HCO that pH value is 8.0~10.53)2Solution is placed in crystallizer, with 1 DEG C/min~5 DEG C/min heating rate
Heated up, meanwhile, it is stirred with 100~500r/min stir speed (S.S.), when mould temperature reaches 60~80 DEG C, to
Mg(HCO3)2Lauryl sodium sulfate is added in solution, wherein, lauryl sodium sulfate addition is Mg (HCO3)2Solution quality
The 1 ‰ of fraction~5 ‰；
After addition is finished, then constant temperature 30~120min of insulation stops heating and stirs, filter, wash, dry, that is, obtain many
The spherical basic carbonate magnesium crystal in hole.
2. the method for preparing porous spherical basic carbonate magnesium crystal using magnesite as claimed in claim 1, it is characterised in that
In described step (1), described calcining, calcining heat is 600~800 DEG C, and calcination time is 1.0~3.0h.
3. the method for preparing porous spherical basic carbonate magnesium crystal using magnesite as claimed in claim 1, it is characterised in that
In described step (2), the temperature of described deionized water is 70~100 DEG C.
4. the method for preparing porous spherical basic carbonate magnesium crystal using magnesite as claimed in claim 1, it is characterised in that
In described step (3), described stirring, its stir speed (S.S.) is 200~500r/min.
5. the method for preparing porous spherical basic carbonate magnesium crystal using magnesite as claimed in claim 1, it is characterised in that
In described step (4), the molar concentration of described NaOH solution is 0.5~2.0mol/L.
6. the method for preparing porous spherical basic carbonate magnesium crystal using magnesite as claimed in claim 1, it is characterised in that
The porous spherical basic carbonate magnesium crystal of preparation, its molecular formula is 4MgCO3·Mg(OH)2·4H2O, its pattern is porous spherical,
The average diameter of porous ball is 4.0~10.0 μm.
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| CN114084894A (en) * | 2021-12-08 | 2022-02-25 | 沈阳理工大学 | Silver willow-shaped porous magnesium carbonate trihydrate crystal synthesized based on glucose and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109052437A (en) * | 2018-09-19 | 2018-12-21 | 常州大学 | A kind of preparation method of the mesoporous magnesia by the molecular floriform appearance of nanoparticle |
| CN109052437B (en) * | 2018-09-19 | 2020-07-07 | 常州大学 | Preparation method of flower-shaped mesoporous magnesium oxide composed of nanoparticles |
| CN109354048A (en) * | 2018-12-13 | 2019-02-19 | 沈阳理工大学 | The method that ionic catalysis magnesite prepares magnesium hydroxide and magnesium carbonate based compound |
| CN109354048B (en) * | 2018-12-13 | 2021-07-27 | 沈阳理工大学 | Method for preparing magnesium hydroxide and magnesium carbonate series compound by ion catalysis of magnesite |
| CN114084894A (en) * | 2021-12-08 | 2022-02-25 | 沈阳理工大学 | Silver willow-shaped porous magnesium carbonate trihydrate crystal synthesized based on glucose and preparation method thereof |
| CN114084894B (en) * | 2021-12-08 | 2023-10-03 | 沈阳理工大学 | Silver Liu Zhuang porous magnesium carbonate trihydrate crystal synthesized based on glucose and preparation method thereof |
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Application publication date: 20171024 |