CN109368672A - A method of prevent Magnesium Hydroxide Nano-particles from reuniting - Google Patents
A method of prevent Magnesium Hydroxide Nano-particles from reuniting Download PDFInfo
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- CN109368672A CN109368672A CN201811564562.3A CN201811564562A CN109368672A CN 109368672 A CN109368672 A CN 109368672A CN 201811564562 A CN201811564562 A CN 201811564562A CN 109368672 A CN109368672 A CN 109368672A
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- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C01F5/14—Magnesium hydroxide
- C01F5/20—Magnesium hydroxide by precipitation from solutions of magnesium salts with ammonia
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- 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
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention discloses a kind of methods for preventing Magnesium Hydroxide Nano-particles from reuniting, and include the following steps: (1) in MgSO4The EDTA dispersing agent that mass percent is 5% and the PEG that mass percent is 1.5% are added in solution, are 11 with the pH value that 15% concentration ammonia precipitation process obtains magnesium hydrate precipitate object and keeps solution；(2) it is that detergent is repeatedly washed or rises distillation with ethyl alcohol azeotropic with the ethyl alcohol of 25% concentration, has then been dried to obtain the Magnesium Hydroxide Nano-particles of anti-agglomeration.This method uses suitable depositing technology, reduces MgSO4Solution concentration and ammonia concn make the pH value in solution be fixed on 11 or so, and the reunion degree that EDTA and PEG etc. can be effectively improved particle is added；Then the dry generation for effectively reducing reunion by rapid draing and at a slow speed；Ethanol washing rises distillation with ethyl alcohol azeotropic and can greatly improve Mg (OH)2Agglomeration.
Description
Technical field
The present invention relates to the technical fields of nano material technique more particularly to one kind to prevent Magnesium Hydroxide Nano-particles from reuniting
Method.
Background technique
A problem during agglomeration is nano-powder preparation and collects.For nano particle since granularity is small, surface is former
Sub- ratio is big, large specific surface area, and surface can be big, is in the unstable shape of energy, thus is easy to coalescence, reunites, and forms secondary grain
Son makes particle diameter become larger, and loses the characteristic that nano particle has, and the preparation and preservation to nano-powder bring very big
It is difficult.In current nano-powder preparation process, prevent particle aggregation as an important process, purpose is exactly to collect grain
Degree narrow distribution, be evenly distributed and soilless sticking bulky grain occur high-purity powder.
There are many factor for influencing powder reunion degree, the group of efficiently reducing including in each step prepared by powder
It is poly- to be just directed to its Crack cause, it adopts an effective measure during the preparation process.It prepares nanometer Mg (OH)2A key technology
Problem is exactly to grasp solution particle to generate one or many agglomerations, and stability wants high, this relates to many
Technology and technological problems need to solve.It is typically prepared Mg (OH)2When be also easy to produce jelly, it is untreated, easily generation particle cluster
Poly- phenomenon.Therefore, when precipitating under suitable conditions, a kind of effective dispersing agent need to be added, so that the Mg (OH) generated2Through surface
It is modified not generate reunion, to steadily exist.Nanometer Mg (OH)2Particle surface adsorbed water molecule forms hydrogen bond ,-OH group
Between easily form liquid phase bridge, cause particle in the drying process strongly combine generate hard aggregation.Therefore, the key of hard aggregation is overcome to exist
In removing hydrone and surface freely unbridged hydroxyl as much as possible.In fact, agglomeration traits run through in the whole process flow,
Therefore solving agglomeration traits is not a simple process.
Summary of the invention
The purpose of the invention is to overcome the above-mentioned prior art, providing one kind prevents Magnesium Hydroxide Nano-particles
The method of reunion, the method for preventing Magnesium Hydroxide Nano-particles from reuniting reduce MgSO using suitable depositing technology4Solution is dense
Degree and ammonia concn make the pH value in solution be fixed on 11 or so, and the reunion journey that EDTA and PEG etc. can be effectively improved particle is added
It spends and makes Mg (OH)2Microscopic appearance be effectively improved；Then by rapid draing and at a slow speed, drying effectively reduces reunion
Occur, Mg (OH)2Drying be divided into two stages, the first stage is that surface moisture vaporizes the control stage, the vaporization of this stage
Moisture is unbound water, and rate of drying is very fast；Second stage is that internal moisture migrates the control stage, which takes
Certainly in material internal moisture to the rate of surface migration, this stage rate of drying is slow；Ethanol washing rises steaming with ethyl alcohol azeotropic
Mg (OH) can greatly be improved by evaporating2Agglomeration.
The technical solution adopted by the present invention to solve the technical problems is: a kind of to prevent Magnesium Hydroxide Nano-particles from reuniting
Method includes the following steps:
(1) in MgSO4The EDTA dispersing agent and mass percent that addition mass percent is 5% in solution are 1.5%
PEG is 11 with the pH value that 15% concentration ammonia precipitation process obtains magnesium hydrate precipitate object and keeps solution；
(2) it is that detergent is repeatedly washed or rises distillation with ethyl alcohol azeotropic with the ethyl alcohol of 25% concentration, then dries
The Magnesium Hydroxide Nano-particles of anti-agglomeration are obtained.
Further, the drying in the step (2) is divided into rapid draing stage and at a slow speed drying stage；Rapid draing
Stage is in 80 DEG C of dry 50min, which is that surface moisture vaporizes the control stage, and the stage moisture of vaporization is
Unbound water, rate of drying are very fast；Drying stage is in 80 DEG C of dry 70min at a slow speed, which is internal water
Divide the migration control stage, which depends on rate of the material internal moisture to surface migration, and rate of drying is slow.
Further, use in the step (2) ethyl alcohol of 25% concentration for detergent to magnesium hydrate precipitate object into
Row repeatedly washing, the Magnesium Hydroxide Nano-particles obtained after dry are nano micro-flake, average grain diameter 20nm.
Further, it is then dried to obtain in the step (2) using distillation is risen with magnesium hydrate precipitate object ethyl alcohol azeotropic
Magnesium Hydroxide Nano-particles be spherical shape, partial size 10nm.
In conclusion the method for preventing Magnesium Hydroxide Nano-particles from reuniting of the invention is using suitable depositing technology, drop
Low MgSO4Solution concentration and ammonia concn make the pH value in solution be fixed on 11 or so, and EDTA and PEG etc., which is added, effectively to be changed
The reunion degree of kind particle simultaneously makes Mg (OH)2Microscopic appearance be effectively improved；Then pass through rapid draing and dry at a slow speed
Effectively reduce the generation of reunion, Mg (OH)2Drying be divided into two stages, the first stage is that surface moisture vaporizes the control stage,
The moisture of this stage vaporization is unbound water, and rate of drying is very fast；Second stage is that internal moisture migrates the control stage, should
Stage rate of drying depends on rate of the material internal moisture to surface migration, this stage rate of drying is slow；Ethanol washing or
Mg (OH) can greatly be improved by rising distillation with ethyl alcohol azeotropic2Agglomeration.
Detailed description of the invention
Fig. 1 is the loss on drying curve graph of magnesium hydroxide；
Fig. 2 be it is surface-modified after magnesium hydroxide SEM figure.
Specific embodiment
Embodiment 1
A kind of method for preventing Magnesium Hydroxide Nano-particles from reuniting, includes the following steps: described in the present embodiment 1
(1) in MgSO4The EDTA dispersing agent and mass percent that addition mass percent is 5% in solution are 1.5%
PEG is 11 with the pH value that 15% concentration ammonia precipitation process obtains magnesium hydrate precipitate object and keeps solution；
(2) it is that detergent is repeatedly washed or rises distillation with ethyl alcohol azeotropic with the ethyl alcohol of 25% concentration, then dries
The Magnesium Hydroxide Nano-particles of anti-agglomeration are obtained.
In the present embodiment, the drying in the step (2) is divided into rapid draing stage and at a slow speed drying stage；Quickly
Drying stage is in 80 DEG C of dry 50min, which is that surface moisture vaporizes control stage, the water of stage vaporization
It is divided into unbound water, rate of drying is very fast；Drying stage is in 80 DEG C of dry 70min at a slow speed, which is interior
Portion's water translocation controls the stage, which depends on rate of the material internal moisture to surface migration, rate of drying
Slowly.
In the present embodiment, using the ethyl alcohol of 25% concentration in the step (2) is detergent to magnesium hydrate precipitate
Object is repeatedly washed, and the Magnesium Hydroxide Nano-particles obtained after dry are nano micro-flake, average grain diameter 20nm.
Or used in step (2) and rise distillation with magnesium hydrate precipitate object ethyl alcohol azeotropic, the nanometer hydrogen being then dried to obtain
Magnesium oxide powder is spherical shape, partial size 10nm.
The combination of complexing agent EDTA and Surfactant PEG can control the crystallization and growth course of magnesium hydroxide.EDTA with
Mg2+Complexing, plays the role of sustained release agent, is conducive to the speed for controlling precipitation from homogeneous solution reaction and nucleus growth；Due in Mg
(OH)2In nucleation and growth course, atom is distributed uneven on different crystal faces, and different crystal faces is caused to inhale EDTA/PEG molecule
Attached quantity is different, these absorption promote or inhibit crystal face by the specific surface energy and growth rate constant for changing crystal face
Growth, and adjustment interface characteristic is to guiding the molecule of organic substrate and inorganic ions in interface regularly arranged to realize nothing
The order of machine crystal nucleation and growth under organic substrate modulation, so as to improve Mg (OH)2The growth uniformity of crystal grain, and
Make its arrangement that there is certain rule, is substantially in the radial growth of extension.With the increase of EDTA/PEG additional amount, magnesium hydroxide
It grows uniformity to increase, but EDTA/PEG additional amount has a threshold values, is greater than 3% when EDTA additional amount is greater than 8%, PEG additional amount
When, particle surface Zeta potential is rapidly reduced to 10mv hereinafter, according to double electrode layer theory, surface potential absolute value less than 20~
Easily reunite between particle when 30mv, is unfavorable for the formation of nanoparticle and grows up.Therefore, EDTA and PEG additional amount be 5% and
It is best when 1.5%.
Dispersing agent is mainly the surface charge distribution for passing through absorption and changing particle, generates electrostatic stabilization and space potential barrier is stablized
Effect is to reach dispersion effect, so selecting suitable dispersing agent is one of the major measure of currently used powder anti-agglomeration.
Nano-sized magnesium hydroxide particle has high surface energy, and it is one that reducing surface area, which reduces Gibbs energy to drop low-surface-energy,
The reason of a spontaneous process, this is also anti-agglomeration and where the shoe pinches.The addition of EDTA is so that Mg (OH)2The satiety of precipitation reaction
Decline with degree, adjusts the surface potential of magnesium hydroxide, improve Mg (OH)2Surface characteristic；And the introducing of PEG makes Mg (OH)2?
The surface of grain can decline, and so that the bonding action of itself and hydrone is weakened or is disappeared, to play the role of anti-agglomeration.
Due to ammonium hydroxide Direct precipitation Mg (OH)2Reaction rate it is very fast, Mg (OH)2Nucleation rate much larger than crystalline substance
Rate of nucleus growing, nucleus have little time to grow up, therefore the nanoparticle granularity generated is very small.Reduce MgSO4Solution concentration and ammonia
Water concentration, and the pH value in solution is made to be fixed on 11 or so, then the reunion of particle can obtain the improvement of different degree of taking advantage of, after dry
Obtained Mg (OH)2Feel is fine and smooth, no harsh feeling, reunion degree very little.
Drying means influences the reunion degree of nano-powder product very big.As shown in Figure 1, magnesium hydroxide 50mins with
It is preceding weightless rapid, illustrate that rate of drying is very fast, weight-loss curve becomes very gentle after 50mins, illustrates that rate of drying compares
It is low.Therefore, the drying process of magnesium hydroxide can be divided into rapid draing and dry two stages at a slow speed.When drying process starts, receive
The bulk temperature of rice magnesium hydroxide is lower than air themperature, and heat passes to magnesium hydroxide by hot-air, makes the temperature of magnesium hydroxide
It increases.With the continuous progress of heat transfer and mass transfer, for nano-sized magnesium hydroxide, moisture content is higher when due to starting, hydrogen-oxygen
Change magnesium internal moisture to be easier to surface migration, the surface of magnesium hydroxide is in wetting state always.The stage rate of drying
Depending on the moisture boil-off rate on magnesium hydroxide surface, so the stage is that surface moisture vaporizes control stage, the vaporization of this stage
Moisture be unbound water.With gradually decreasing for magnesium hydroxide moisture content, cause moisture from inside magnesium hydroxide body phase
It is less than the boil-off rate of magnesium hydroxide surface moisture to the rate of surface migration, therefore the stage rate of drying depends in material
Portion's moisture is to the rate of surface migration, so the stage is the internal moisture migration control stage, thus this stage rate of drying is slow.
It in order to accelerate rate of drying, and prevents magnesium hydroxide from reuniting in the drying process, above-described embodiment side can be used
The dry magnesium hydroxide of two kinds of drying modes of formula: it a) is dried in drying box after for several times with ethanol washing；B) it is risen with ethyl alcohol azeotropic
Distill drying.It is fluffy with sample dry after ethanol washing, it is nano micro-flake, average grain diameter 20nm or so；And with ethyl alcohol azeotropic
The dry magnesium hydroxide sample granularity of the method for distillation is minimum, and only 10nm or so, pattern is based on spherical shape.
In addition, the water in sediment is one of the factor for causing nanoparticle to be reunited, therefore use washing methods appropriate
Washing in sediment is gone to be the major way for preventing nanoparticle from reuniting.It is sufficiently washed with the small organic solvent of surface tension
Nano particle can replace the moisture of particle surface absorption, reduce the effect of hydrogen bond, reduce the capillary force of particle coalescence, make
Particle is no longer reunited.It uses ethyl alcohol for detergent, Mg (OH) can be washed away2The water of coordination molecule of particle surface, ethanol molecule can
To replace Mg (OH)2The hydrone of absorption is replaced the hydroxyl groups of particle surface with alkoxy, and then reduces Mg (OH)2Surface
Polarity makes Mg (OH)2In the drying process will not because of hydrogen bond effect and bond reunion, while improving rate of drying, make
The hydroxide nanoparticle microplate of generation will not because of the contracting shell mechanism in drying breaks up agglomerations, it is micro- to be conducive to small nano magnesia
The formation of piece with grow up.And ethyl alcohol azeotropic distillation method can also effectively reduce particle aggregation.Tradition is such as used directly to dry with drying box
The product of dry (without using ethanol washing or azeotropic distillation) is reunited seriously, and is hard aggregation, and particle is micron order.
As shown in Fig. 2, nano micro-flake continuity is preferable, lamella area is larger, and width is 0.5 μm or so, with a thickness of 25nm
Left and right, growth is more uniform, and arrangement has certain rule and orientation, and basic is in the radial growth of extension.Obviously, EDTA with
PEG molecule plays an important role the formation of hydroxide nanoparticle microplate and growing up, EDTA and PEG molecular Control magnesium hydroxide
The formation and growth rate of nucleus, adjust the interfacial characteristics of nucleus to guide magnesium hydroxide grain orientation to grow, limitation and
The growth behavior of specification magnesium hydroxide crystal grain enables the nano micro-flake with certain oriented growth of homoepitaxial to be formed.
The above described is only a preferred embodiment of the present invention, not making any form to technical solution of the present invention
On limitation.According to the technical essence of the invention any simple modification to the above embodiments, equivalent variations and repair
Decorations, in the range of still falling within technical solution of the present invention.
Claims (4)
1. a kind of method for preventing Magnesium Hydroxide Nano-particles from reuniting, which comprises the steps of:
(1) in MgSO4The EDTA dispersing agent that mass percent is 5% and the PEG that mass percent is 1.5% are added in solution, are used
15% concentration ammonia precipitation process obtains magnesium hydrate precipitate object and keeps the pH value of solution to be 11；
(2) it is that detergent is repeatedly washed or rises distillation with ethyl alcohol azeotropic with the ethyl alcohol of 25% concentration, is then dried to obtain
The Magnesium Hydroxide Nano-particles of anti-agglomeration.
2. a kind of method for preventing Magnesium Hydroxide Nano-particles from reuniting according to claim 1, which is characterized in that described
Drying in step (2) is divided into rapid draing stage and at a slow speed drying stage；The rapid draing stage be in 80 DEG C of dry 50min,
The rapid draing stage be surface moisture vaporize the control stage, the stage vaporization moisture be unbound water, rate of drying compared with
Fastly；Drying stage is in 80 DEG C of dry 70min at a slow speed, which is that internal moisture migrates control stage, the stage
Rate of drying depends on rate of the material internal moisture to surface migration, and rate of drying is slow.
3. a kind of method for preventing Magnesium Hydroxide Nano-particles from reuniting according to claim 2, which is characterized in that described
It uses the ethyl alcohol of 25% concentration repeatedly to be washed for detergent to magnesium hydrate precipitate object in step (2), is obtained after dry
Magnesium Hydroxide Nano-particles are nano micro-flake, average grain diameter 20nm.
4. a kind of method for preventing Magnesium Hydroxide Nano-particles from reuniting according to claim 2, which is characterized in that the step
Suddenly using distillation is risen with magnesium hydrate precipitate object ethyl alcohol azeotropic in (2), the Magnesium Hydroxide Nano-particles being then dried to obtain are ball
Shape, partial size 10nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110152058A (en) * | 2019-05-31 | 2019-08-23 | 北京幸福益生再生医学科技有限公司 | A kind of regenerative medicine material and preparation method thereof |
| CN110954450A (en) * | 2019-12-02 | 2020-04-03 | 江苏厚生新能源科技有限公司 | Test method for improving particle size of alumina slurry |
| CN111943215A (en) * | 2019-05-14 | 2020-11-17 | 中天科技精密材料有限公司 | Preparation method of quartz powder |
-
2018
- 2018-12-20 CN CN201811564562.3A patent/CN109368672A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111943215A (en) * | 2019-05-14 | 2020-11-17 | 中天科技精密材料有限公司 | Preparation method of quartz powder |
| CN111943215B (en) * | 2019-05-14 | 2022-02-22 | 中天科技精密材料有限公司 | Preparation method of quartz powder |
| CN110152058A (en) * | 2019-05-31 | 2019-08-23 | 北京幸福益生再生医学科技有限公司 | A kind of regenerative medicine material and preparation method thereof |
| CN110954450A (en) * | 2019-12-02 | 2020-04-03 | 江苏厚生新能源科技有限公司 | Test method for improving particle size of alumina slurry |
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Application publication date: 20190222 |