CN106348251A - Method for preparing monodisperse oxide nanoparticles - Google Patents
Method for preparing monodisperse oxide nanoparticles Download PDFInfo
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- CN106348251A CN106348251A CN201610699775.1A CN201610699775A CN106348251A CN 106348251 A CN106348251 A CN 106348251A CN 201610699775 A CN201610699775 A CN 201610699775A CN 106348251 A CN106348251 A CN 106348251A
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- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/18—Methods for preparing oxides or hydroxides in general by thermal decomposition of compounds, e.g. of salts or hydroxides
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Abstract
The invention discloses a method for preparing monodisperse oxide nanoparticles. The method comprises the steps of firstly, preparing hydrosol containing a soluble salt and a nano-oxide precursor, then, mixing the hydrosol with a low-polarity solvent so as to precipitate the soluble salt in a superfine nanoparticle state and co-precipitate the soluble salt with nano-oxide precursor particles, subjecting the co-precipitate to centrifugation, washing and drying, carrying out calcination at a temperature below the boiling point of the salt so as to convert the nano-oxide precursor into a nano oxide, washing off the soluble salt, and carrying out drying, thereby obtaining the monodisperse oxide nanoparticles. During the preparation, the soluble salt exerts an isolating action, and the precursor nanoparticles or oxide nanoparticles can be effectively prevented from agglomeration and sintering in a high-temperature calcination process. According to the method, the temperature range for preparing monodisperse nano-oxides is widened greatly, and the process is simple and convenient and is low in cost.
Description
Technical field
The invention belongs to field of nano material preparation, it is related to a kind of method preparing dispersed nano oxide particle.
Background technology
Nano-oxide particles refer generally to superfine oxide particle between 1-100nm for the size.Nano-oxide due to
There is quantum size effect, bulk effect, skin effect and tunnel-effect, in calorifics, optics, electricity, magnetics and chemistry side
Face has very unique property, is therefore used widely.
The preparation method of nano-oxide particles has sol-gal process, chemical precipitation method, microemulsion method, hydro-thermal method, spraying
Pyrolysismethod etc., the basic process of these preparation methoies is all to prepare oxide precursor first, then by presoma in high temperature
Lower calcining and decomposing, obtains nano-oxide.It is difficult to solve reunion and the burning of nano-particle in the preparation process of nano-oxide
Knot problem.Because nano particles are little, surface energy is big, is in energy labile state, tiny granule trends towards being gathered in
Together.In drying and high-temperature burning process, easily sinter between granule.But high-temperature burning process is often difficult to avoid that,
As prepared aluminium oxide using aluminium hydroxide or aluminium carbonate ammonium decomposition method, need to calcine more than 200 DEG C, γ type aluminium oxide is changed into
Alpha-type aluminum oxide needs to calcine more than 1000 DEG C；Basic magnesium carbonate decomposition method prepares magnesium oxide, needs through more than 500 DEG C
High-temperature calcination；And lanthanum hydroxide decomposites the temperature of lanthana at 750 DEG C about；Anatase titanium dioxide is more than 600 DEG C
It is changed into rutile-type.In high-temperature burning process, nano-particle will produce serious sintering it is difficult to obtain mono-dispersed nano
Oxide particle.
Chinese invention patent cn201610365324.4 proposes and a kind of coats solubility salt crust in nano grain surface
Method, in calcination process, salt crust plays buffer action, the later stage removes it again, can be prevented effectively from nano-particle at high temperature
Reunite and sinter, obtain dispersed nano compound particle.But the method complex process, cost of raw material height and low yield.In
State's patent of invention cn201410047796.6 proposes a kind of side preparing single dispersion metal or monocrystalline metal oxide nano-particle
Method, the water in oil microemulsion containing alkali halide is carried out azeotropic distillation, obtains the metal of alkali halide parcel
Presoma nano-particle, then carry out calcining, wash and obtain nano-particle.The method equally exists cost of raw material height and yields poorly
Shortcoming, azeotropic distillation process is complicated simultaneously, vapo(u)rizing temperature is high, and the stability of microemulsion is difficult to ensure that.
In sum, being isolated using soluble-salt is to solve the problems, such as nano-particle high temperature sintering, prepare dispersed nano oxygen
One possible approaches of compound granule, but existing soluble-salt isolation technology all to there is complex process, high cost, yield low
Shortcoming.Find a kind of method preparing dispersed nano granule of Cheap highly effective, nano material preparation technology development is had
Important meaning.
Content of the invention
Technical problem: the invention provides one kind can solve the problems, such as nano-particle high temperature sintering, fast and convenient and yield is high
The method preparing dispersed nano oxide particle.
Technical scheme: a kind of method preparing dispersed nano oxide particle that the present invention provides, comprise the following steps:
1) soluble-salt is dissolved in the hydrosol of nano-oxide presoma；
2) the described hydrosol is mixed with weak polar solvent, so that soluble-salt is separated out with superfine nano graininess, and with
Nano-oxide granular precursor co-precipitation；
3) by described step 2) centrifugation of the precipitate that obtains, washing, it is dried, calcine below soluble-salt boiling point；
4) deionized water washes the soluble-salt in calcined product off, can obtain dispersed nano oxide particle after being dried.
Further, in the inventive method, nano-oxide presoma is the presoma of following nano-oxide: oxidation
Aluminum, titanium oxide, ferrum oxide, magnesium oxide, zirconium oxide, copper oxide, nickel oxide, stannum oxide, Indium sesquioxide., yittrium oxide, europium oxide, oxidation
Cerium, lanthana, terbia. Diterbium trioxide, dysprosia or Dineodymium trioxide.
Further, in the inventive method, soluble-salt refers to sodium chloride, potassium chloride, sodium bromide, potassium bromide, sodium sulfate
Or potassium sulfate.
Further, in the inventive method, described nano-oxide presoma is the hydration oxygen corresponding to nano-oxide
Compound, carbonate, ammonium carbonate salts or subcarbonate, described nano-oxide presoma is water insoluble and can decompose at high temperature
Generate or be converted into nano-oxide.
Further, in the inventive method, nano-oxide presoma is γ type nano aluminium oxide, described γ type nano oxygen
Change aluminum and can be converted into α type nano aluminium oxide more than 1000 DEG C.
Further, in the inventive method, nano-oxide presoma is anatase-type nanometer titanium dioxide, described sharp titanium
Ore deposit type nano titanium oxide can be converted into rutile titanium dioxide more than 600 DEG C.
Further, in the inventive method, nano-oxide presoma is γ type nano-sized iron oxide, described γ type nano oxygen
Change ferrum and can be converted into α type nano-sized iron oxide more than 400 DEG C.
Further, in the inventive method, in the hydrosol, the mass ratio of soluble-salt and nano-oxide presoma >=
0.05.
Further, in the inventive method, weak polar solvent is acetone, methanol, ethanol, propanol, isopropanol or the tert-butyl alcohol.
Further, in the inventive method, the hydrosol of nano-oxide presoma refers to by a diameter of 1-100nm's
Nano-oxide granular precursor is dispersed in water obtained colloid.
Further, in the inventive method, in the hydrosol, generally also contain surfactant, including Polyethylene Glycol (peg),
Polyvinylpyrrolidone (pvp), polyvinyl alcohol (pva), cetyl trimethylammonium bromide (ctab), cetyl trimethyl chlorine
Change ammonium (ctac), dodecyl alanine, dodecyldimethylammonium hydroxide inner salt, gelatin or natural gum.
The present invention prepares the hydrosol containing soluble-salt and nano-oxide presoma first, then by this hydrosol with weak
Polar solvent mix, separate out tiny nanometer salt particle, and with nano-oxide granular precursor co-precipitation, by co-precipitate from
The heart, washing, drying, calcine below salt boiling point, make nano-oxide presoma be changed into nano-oxide, wash away solubility
Salt, can obtain mono-dispersed nano oxide particle after being dried.In the process, soluble-salt plays buffer action, can effectively keep away
Exempt from the reunion in high-temperature burning process of nanometer granular precursor or nano-oxide particles and sintering.
Beneficial effect: the present invention compared with prior art, has the advantage that
The method comprises the steps of firstly, preparing the hydrosol containing soluble-salt and nano-oxide presoma, then by the hydrosol with weak
Polar solvent mixes, and so that soluble-salt is separated out from water with the state of tiny nano-particle and surround nano-oxide presoma
Granule.Meanwhile the stability of the hydrosol is destroyed, and therefore nanometer salt particle is wrapped in nano-oxide granular precursor together
When precipitation.Because nanometer granular precursor is isolated by salt, nanometer granular precursor or nano-oxide therefore can be prevented effectively from
Reunion in high-temperature burning process for the grain and sintering.Calcined product is washed, be dried after can obtain mono-dispersed nano oxide
Grain.The present invention has widened the temperature range preparing dispersed nano oxide significantly, and simple process, low cost, yield are high.
The hydrous oxide corresponding to oxide in the inventive method, carbonate, ammonium carbonate salts or subcarbonate, γ
Type nano aluminium oxide, anatase-type nanometer titanium dioxide and γ type nano-sized iron oxide are easy to make the grain of a diameter of 1-100nm
Son, and colloid solution can be dispersed in water, or claim the hydrosol.Can be made into Alumina gel as hydrated alumina, Yttrium trihydroxide can be made
Yttrium colloidal sol, anatase-type nanometer titanium dioxide is become to can be made into titanium colloidal sol etc..In the hydrosol, generally also contain surfactant,
As Polyethylene Glycol (peg), Polyvinylpyrrolidone (pvp), polyvinyl alcohol (pva), cetyl trimethylammonium bromide (ctab),
Hexadecyltrimethylammonium chloride (ctac), dodecyl alanine, dodecyldimethylammonium hydroxide inner salt, gelatin and natural gum
Deng making the hydrosol more stable.
Soluble-salt in the inventive method is alkali halide or alkali metal sulfates, is added to as electrolyte
In the hydrosol.Alkali halide is electrolyzed to produce alkali metal cation and halogen anion after adding the hydrosol, obtains containing solvable
The transparent hydrosol of property salt.Because the coagulation ability of alkali metal cation and halogen anion is very weak, even if alkali halide
The higher coagulation also not resulting in colloidal particle of content of salt.As added sodium chloride salt in Alumina gel, even if reaching sodium chloride
Saturated concentration be also not result in Alumina gel occur coagulation, and still be transparent clear colloidal.Even if add in the hydrosol is
Alkali metal sulfates, in the range of finite concentration, the hydrosol can also keep stable.When in colloid contain peg, pvp, pva etc.
During surfactant, in colloid, the content of salt can be higher.
Nano-oxide granular precursor in the hydrosol has the ability of very strong adion, and therefore colloidal particle is deposited
In double electrical layerses, i.e. close bed and diffusion layer.Nano-oxide granular precursor is referred to as glue core, if glue core absorption cation band
Positive electricity, positively charged colloidal particle will adsorb anion again further.Part anion enters close bed, structure together with glue core
Become " micelle ", other anion are located at diffusion layer.Glue core, close bed are constituted " micelle " together with diffusion layer ion.Whole glue
Group is electroneutral that is to say, that in the hydrosol containing electrolyte, the cation that electrolyte ionizes out and anion are all rich
Collection is around nano-oxide presoma glue core.
If the hydrosol heating evaporation that this is contained soluble-salt and nano-oxide presoma, soluble-salt can be made to crystallize
Separate out, but the salt particle separating out is thick, nanometer presoma nano-particle will be attached to around thick salt particle it is difficult to realize salt
Granule isolates the purpose of granular precursor, can reunite simultaneously, be finally difficult to obtain between nano-oxide granular precursor
Monodisperse particles.We have discovered that, when this hydrosol containing soluble-salt is mixed with weak polar solvent, with the hydrosol
The change of polarity, soluble-salt moment is separated out from water with the state of tiny nano-particle, and the nm salt particle size of precipitation is non-
Often tiny, diameter only 1-3nm, less than the size of nano-oxide granular precursor.The tiny nanometer salt particle separating out surrounds simultaneously
Isolation nano-oxide granular precursor.Meanwhile the stability of the hydrosol is destroyed, nanometer salt particle and oxide precursor
Body granule precipitates simultaneously.Nanometer salt particle is wrapped in around nano-oxide granular precursor, if nano-oxide presoma
Size be 40nm, nanometer salt particle is 2nm, can be real when the volume ratio of salt particle and oxide precursor is 0.15 about
Existing nanometer salt particle is to the parcel of nano-oxide granular precursor and isolation.When the size of nano-oxide presoma is bigger,
Or nanometer salt particle smaller when, required salt particle is then less with the volume ratio of nano-oxide presoma.
The fusing point of soluble-salt used by the present invention is higher, such as up to 801 DEG C of the fusing point of sodium chloride, and the fusing point of potassium sulfate is up to
1069℃.When co-precipitate is calcined under salt fusing point, decomposed, will not sinter between nano-particle, therefore will calcine
Mono-dispersed nano oxide particle can be obtained after product washing.
When co-precipitate more than salt fusing point, below boiling point calcine when, nano-particle can occur a certain degree of ripening and
Grow up, but under the isolation of fused salt, still can keep monodisperse status, be still dispersed nano oxide after calcined product washing
Grain.Nano-oxide particles are grown up degree and this oxide dissolubility in fused salt and temperature of molten salt in the ripening in fused salt
Relevant etc. factor, when dissolubility is less, nano-particle can't substantially be grown up.If nano aluminium oxide is in 1000 DEG C of potassium chloride fused salts
In change in particle size very slow, but change in particle size in 1100 DEG C of sodium chloride fused salts for the nano magnesia is very fast.
The invention has the advantages that 1, soluble-salt and nano-oxide presoma co-precipitation can be made, and by oxide
Granular precursor is isolated, and when being allowed to calcining and decomposing under salt boiling point, still keeps monodispersity；2, present invention process is easy, one-tenth
This is cheap, extremely low to equipment requirements；3, universality is strong, is not only widely used in the system of water-fast nano-oxide particles
Standby, it is also applied for the preparation of other water-fast nano-particle, nano-particle can also be improved using the art of this patent
Crystallinity.
Specific embodiment
Below the preferred embodiments of the invention are elaborated.
In the present invention, water-soluble salt all can use as isolated material.Example for the soluble-salt of the present invention
Sodium chloride, potassium chloride, lithium chloride, cesium chloride, Rubinorm (Ifi)., lithium sulfate, sodium sulfate, potassium sulfate, cesium sulfate, sulphuric acid can be included
Rubidium, sodium bromide, potassium bromide, lithium bromide, lithium fluoride, sodium fluoride, potassium fluoride, sodium phosphate, sodium metaaluminate, sodium nitrate, potassium nitrate, carbon
Sour sodium, potassium carbonate.From the point of view of stability, cost and boiling point, preferably use sodium chloride, potassium chloride, sodium bromide, bromination
Potassium, sodium sulfate or potassium sulfate.
In the present invention, there is not chemical reaction and the water-fast nano oxygen of its presoma with water and selected salt
Compound granule all can be suitable for.Nano-oxide for the present invention can be silicon oxide, magnesium oxide, aluminium oxide, titanium oxide, oxidation
Ferrum, zirconium oxide, copper oxide, nickel oxide, niobium oxide, stannum oxide, Indium sesquioxide., yittrium oxide, europium oxide, cerium oxide, lanthana, oxidation
Terbium, dysprosia or Dineodymium trioxide.From the point of view of stability, preferably use magnesium oxide, aluminium oxide, titanium oxide, ferrum oxide, oxidation
Zirconium, copper oxide, nickel oxide, stannum oxide, Indium sesquioxide., yittrium oxide, europium oxide, cerium oxide, lanthana, terbia. Diterbium trioxide, dysprosia or oxygen
Change neodymium.
In the present invention, water insoluble and at high temperature decomposable asymmetric choice net generate or be converted into the presoma of oxide and all can be suitable for.
Oxide precursor for the present invention can be that decomposable asymmetric choice net generates the hydrous oxide of this oxide, carbonic acid in high-temperature calcination
Salt, ammonium carbonate salts or subcarbonate.
In the present invention, oxide precursor can also be the low temperature phase oxide that crystal conversion occurs under high temperature, including γ
Type aluminium oxide, anatase titanium dioxide and γ type ferrum oxide.Wherein γ type aluminium oxide is changed into the oxidation of α type more than 1000 DEG C
Aluminum, anatase titanium dioxide is changed into rutile titanium dioxide more than 600 DEG C, and γ type ferrum oxide turns more than 400 DEG C
It is changed into α type ferrum oxide.
In the present invention, generally also contain surfactant in the hydrosol, including Polyethylene Glycol (peg), polyvinylpyrrolidine
Ketone (pvp), polyvinyl alcohol (pva), cetyl trimethylammonium bromide (ctab), hexadecyltrimethylammonium chloride (ctac),
Dodecyl alanine, dodecyldimethylammonium hydroxide inner salt, gelatin or natural gum.
In the present invention, polarity is less than water and can solvent miscible with water all can use.Weak polar solvent for the present invention
Example can include for pyridine, dioxanes, oxolane, acetone, methanol, ethanol, isopropanol or the tert-butyl alcohol.Chemically stable
From the point of view of property and avirulence, preferably acetone, methanol, ethanol, propanol, isopropanol or the tert-butyl alcohol.Receive for improving in the hydrosol
The sedimentation fraction of rice oxide precursor granule, can add appropriate flocculant or alkali in weak polar solvent.
Below in conjunction with specific embodiment, the preparation method of the present invention is further elaborated with.
Embodiment 1
Take 3 grams of the algeldrate hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add hydrated hydroxide
Change in the aluminum hydrosol, ultrasonic disperse becomes the transparent Alumina gel containing sodium chloride.This Alumina gel is mixed with 5 milliliters of dehydrated alcohol,
Precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, be washed with deionized water after cooling
Fall sodium chloride salt, after being dried, dispersed nano aluminium oxide can be obtained.
Embodiment 2
Take 3 grams of the algeldrate hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium sulfate, add hydrated hydroxide
Change in the aluminum hydrosol, ultrasonic disperse becomes the transparent Alumina gel containing sodium sulfate.This Alumina gel is mixed with 5 milliliters of dehydrated alcohol,
Precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 800 DEG C, be washed with deionized water after cooling
Fall sodium sulfate salt, after being dried, dispersed nano aluminium oxide can be obtained.
Embodiment 3
Take 3 grams of the algeldrate hydrosol containing 10% weight ratio, weigh 0.3 gram of potassium sulfate, add hydrated hydroxide
Change in the aluminum hydrosol, ultrasonic disperse becomes the transparent Alumina gel containing potassium sulfate.This Alumina gel is mixed with 5 milliliters of dehydrated alcohol,
Precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 1000 DEG C, deionized water after cooling
Wash potassium sulfate salt off, after being dried, dispersed nano aluminium oxide can be obtained.
Embodiment 4
Take 3 grams of the algeldrate hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium bromide, add hydrated hydroxide
Change in the aluminum hydrosol, ultrasonic disperse becomes the transparent Alumina gel containing sodium bromide.This Alumina gel is mixed with 5 milliliters of dehydrated alcohol,
Precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 700 DEG C, be washed with deionized water after cooling
Fall bromination sodium salt, after being dried, dispersed nano aluminium oxide can be obtained.
Embodiment 5
Take 3 grams of the algeldrate hydrosol containing 10% weight ratio, weigh 0.6 gram of potassium bromide, add hydrated hydroxide
Change in the aluminum hydrosol, ultrasonic disperse becomes the transparent Alumina gel containing potassium bromide.This Alumina gel is mixed with 5 milliliters of dehydrated alcohol,
Precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 700 DEG C, be washed with deionized water after cooling
Fall bromination potassium salt, after being dried, dispersed nano aluminium oxide can be obtained.
Embodiment 6
Take 3 grams of the titanium hydroxide hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add titanium hydroxide water-soluble
In glue, ultrasonic disperse becomes the transparent titanium hydroxide colloidal sol containing sodium chloride.This titanium hydroxide colloidal sol is mixed with 5 milliliters of dehydrated alcohol
Close, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, after cooling, use deionization
Water-wash away sodium chloride salt, after being dried, dispersed nano titanium oxide can be obtained.
Embodiment 7
Take 3 grams of the magnesium hydroxide hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add magnesium hydroxide colloidal sol
In, ultrasonic disperse becomes the transparent magnesium hydroxide colloidal sol containing sodium chloride.This magnesium hydroxide colloidal sol is mixed with 5 milliliters of dehydrated alcohol
Close, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, after cooling, use deionization
Water-wash away sodium chloride salt, after being dried, dispersed nano magnesium oxide can be obtained.
Embodiment 8
Take 3 grams of the hydrated ferric oxide. hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add ferric hydroxide sol
In, ultrasonic disperse becomes the transparent ferric hydroxide sol containing sodium chloride.This ferric hydroxide sol is mixed with 5 milliliters of dehydrated alcohol
Close, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, after cooling, use deionization
Water-wash away sodium chloride salt, after being dried, dispersed nano ferrum oxide can be obtained.
Embodiment 9
Take 3 grams of the zirconium hydroxide hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add zirconium hydroxide water-soluble
In glue, ultrasonic disperse becomes the transparent zirconium hydroxide sols containing sodium chloride.This zirconium hydroxide sols is mixed with 5 milliliters of dehydrated alcohol
Close, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, after cooling, use deionization
Water-wash away sodium chloride salt, after being dried, dispersed nano zirconium oxide can be obtained.
Embodiment 10
Take 3 grams of the Copper hydrate hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add Copper hydrate water-soluble
In glue, ultrasonic disperse becomes the transparent Copper hydrate colloidal sol containing sodium chloride.This Copper hydrate colloidal sol is mixed with 5 milliliters of dehydrated alcohol
Close, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, after cooling, use deionization
Water-wash away sodium chloride salt, after being dried, dispersed nano copper oxide can be obtained.
Embodiment 11
Take 3 grams of the stannic hydroxide hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, the hydro-oxidation stannum hydrosol
In, ultrasonic disperse becomes the transparent stannic hydroxide colloidal sol containing sodium chloride.This stannic hydroxide colloidal sol is mixed with 5 milliliters of dehydrated alcohol
Close, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, after cooling, use deionization
Water-wash away sodium chloride salt, after being dried, dispersed nano stannum oxide can be obtained.
Embodiment 12
Take 3 grams of the indium hydroxide hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add indium hydroxide water-soluble
In glue, ultrasonic disperse becomes the transparent indium hydroxide colloidal sol containing sodium chloride.This indium hydroxide colloidal sol is mixed with 5 milliliters of dehydrated alcohol
Close, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, after cooling, use deionization
Water-wash away sodium chloride salt, after being dried, dispersed nano Indium sesquioxide. can be obtained.
Embodiment 13
Take 3 grams of the Yttrium trihydroxide hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add Yttrium trihydroxide water-soluble
In glue, ultrasonic disperse becomes the transparent Yttrium trihydroxide colloidal sol containing sodium chloride.This Yttrium trihydroxide colloidal sol is mixed with 5 milliliters of dehydrated alcohol
Close, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, after cooling, use deionization
Water-wash away sodium chloride salt, after being dried, dispersed nano yittrium oxide can be obtained.
Embodiment 14
Take 3 grams of the cerium hydroxide hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add cerium hydroxide water-soluble
In glue, ultrasonic disperse becomes the transparent cerium hydroxide sol containing sodium chloride.This cerium hydroxide sol is mixed with 5 milliliters of dehydrated alcohol
Close, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, after cooling, use deionization
Water-wash away sodium chloride salt, after being dried, dispersed nano cerium oxide can be obtained.
Embodiment 15
Take 3 grams of the lanthanum hydroxide hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add lanthanum hydroxide water-soluble
In glue, ultrasonic disperse becomes the transparent lanthanum hydroxide colloidal sol containing sodium chloride.This lanthanum hydroxide colloidal sol is mixed with 5 milliliters of dehydrated alcohol
Close, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 780 DEG C, after cooling, use deionization
Water-wash away sodium chloride salt, after being dried, dispersed nano lanthana can be obtained.
Embodiment 16
Take 3 grams of the terbium hydroxide hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add terbium hydroxide water-soluble
In glue, ultrasonic disperse becomes the transparent terbium hydroxide colloidal sol containing sodium chloride.This terbium hydroxide colloidal sol is mixed with 5 milliliters of dehydrated alcohol
Close, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, after cooling, use deionization
Water-wash away sodium chloride salt, after being dried, dispersed nano terbia. Diterbium trioxide can be obtained.
Embodiment 17
Take 3 grams of the Dysprosium hydroxide hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add Dysprosium hydroxide water-soluble
In glue, ultrasonic disperse becomes the transparent Dysprosium hydroxide colloidal sol containing sodium chloride.This Dysprosium hydroxide colloidal sol is mixed with 5 milliliters of dehydrated alcohol
Close, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, after cooling, use deionization
Water-wash away sodium chloride salt, after being dried, dispersed nano dysprosia can be obtained.
Embodiment 18
Take 3 grams of the Neodymium hydroxide hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add Neodymium hydroxide water-soluble
In glue, ultrasonic disperse becomes the transparent Neodymium hydroxide colloidal sol containing sodium chloride.This Neodymium hydroxide colloidal sol is mixed with 5 milliliters of dehydrated alcohol
Close, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, after cooling, use deionization
Water-wash away sodium chloride salt, after being dried, dispersed nano Dineodymium trioxide can be obtained.
Embodiment 19
Take 2 grams of the Yttrium trihydroxide hydrosol containing 40% weight ratio, weigh 0.04 gram of sodium chloride, add Yttrium trihydroxide water-soluble
In glue, ultrasonic disperse becomes the transparent Yttrium trihydroxide colloidal sol containing sodium chloride.This Yttrium trihydroxide colloidal sol is mixed with 5 milliliters of dehydrated alcohol
Close, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, after cooling, use deionization
Water-wash away sodium chloride salt, after being dried, dispersed nano yittrium oxide can be obtained.
Embodiment 20
Take 3 grams of the Yttrium trihydroxide hydrosol containing 30% weight ratio, weigh 0.9 gram of sodium chloride, add Yttrium trihydroxide water-soluble
In glue, ultrasonic disperse becomes the transparent Yttrium trihydroxide colloidal sol containing sodium chloride.This Yttrium trihydroxide colloidal sol is mixed with 5 milliliters of dehydrated alcohol
Close, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, after cooling, use deionization
Water-wash away sodium chloride salt, after being dried, dispersed nano yittrium oxide can be obtained.
Embodiment 21
Take 3 grams of the hydrated ferric oxide. hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add hydronium(ion) ferrum oxide
In the hydrosol, ultrasonic disperse becomes the transparent ferric hydroxide sol containing sodium chloride.This ferric hydroxide sol is mixed with 5 milliliters of acetone
Close, precipitate is centrifuged, uses acetone supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, be washed with deionized water after cooling
Fall sodium chloride salt, after being dried, dispersed nano ferrum oxide can be obtained.
Embodiment 22
Take 3 grams of the hydrated ferric oxide. hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add hydronium(ion) ferrum oxide
In the hydrosol, ultrasonic disperse becomes the transparent ferric hydroxide sol containing sodium chloride.This ferric hydroxide sol is mixed with 5 ml methanol
Close, precipitate is centrifuged, uses methanol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, be washed with deionized water after cooling
Fall sodium chloride salt, after being dried, dispersed nano ferrum oxide can be obtained.
Embodiment 23
Take 3 grams of the hydrated ferric oxide. hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add hydronium(ion) ferrum oxide
In the hydrosol, ultrasonic disperse becomes the transparent ferric hydroxide sol containing sodium chloride.This ferric hydroxide sol is mixed with 5 milliliters of propanol
Close, precipitate is centrifuged, uses propanol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, be washed with deionized water after cooling
Fall sodium chloride salt, after being dried, dispersed nano ferrum oxide can be obtained.
Embodiment 24
Take 3 grams of the hydrated ferric oxide. hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add hydronium(ion) ferrum oxide
In the hydrosol, ultrasonic disperse becomes the transparent ferric hydroxide sol containing sodium chloride.By this ferric hydroxide sol and 5 milliliters of isopropanols
Mixing, precipitate is centrifuged, uses isopropanol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, use deionization after cooling
Water-wash away sodium chloride salt, after being dried, dispersed nano ferrum oxide can be obtained.
Embodiment 25
Take 3 grams of the hydrated ferric oxide. hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add hydronium(ion) ferrum oxide
In the hydrosol, ultrasonic disperse becomes the transparent ferric hydroxide sol containing sodium chloride.By this ferric hydroxide sol and 5 milliliters of tert-butyl alcohols
Mixing, precipitate is centrifuged, uses tert-butyl alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, use deionization after cooling
Water-wash away sodium chloride salt, after being dried, dispersed nano ferrum oxide can be obtained.
Embodiment 26
Take 3 grams of the algeldrate hydrosol containing 10% weight ratio, weigh 0.6 gram of potassium chloride, add hydrated hydroxide
Change in the aluminum hydrosol, ultrasonic disperse becomes the transparent Alumina gel containing potassium chloride.This Alumina gel is mixed with 5 milliliters of dehydrated alcohol,
Precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 1200 DEG C, deionized water after cooling
Wash potassium chloride salt off, after being dried, single dispersing α type nano aluminium oxide can be obtained.
Embodiment 27
Take 3 grams of the algeldrate hydrosol containing 10% weight ratio, weigh 0.6 gram of potassium chloride, add hydrated hydroxide
Change in the aluminum hydrosol, ultrasonic disperse becomes the transparent Alumina gel containing potassium chloride.This Alumina gel is mixed with 5 milliliters of dehydrated alcohol,
Precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 30 minutes at 1300 DEG C, deionized water after cooling
Wash potassium chloride salt off, after being dried, single dispersing α type nano aluminium oxide can be obtained.
Embodiment 28
Take 3 grams of the algeldrate hydrosol containing 10% weight ratio, weigh 0.9 gram of sodium chloride, add hydrated hydroxide
Change in the aluminum hydrosol, ultrasonic disperse becomes the transparent hydration aluminum hydroxide sol containing sodium chloride.By this algeldrate colloidal sol
Mix with 5 milliliters of dehydrated alcohol, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, little in 750 DEG C of calcinings 1
When, after cooling, deionized water washes sodium chloride salt off, can obtain dispersed nano aluminium oxide after being dried.
Embodiment 29
Take 3 grams of the algeldrate hydrosol containing 5% weight ratio, weigh 0.9 gram of sodium chloride, add hydronium(ion) oxidation
In the aluminum hydrosol, ultrasonic disperse becomes the transparent hydration aluminum hydroxide sol containing sodium chloride.By this algeldrate colloidal sol and 5
Milliliter dehydrated alcohol mixing, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C,
After cooling, deionized water washes sodium chloride salt off, can obtain dispersed nano aluminium oxide after being dried.
Embodiment 30
Take 3 grams of the algeldrate hydrosol containing 3% weight ratio, weigh 0.9 gram of sodium chloride, add hydronium(ion) oxidation
In the aluminum hydrosol, ultrasonic disperse becomes the transparent hydration aluminum hydroxide sol containing sodium chloride.By this algeldrate colloidal sol and 5
Milliliter dehydrated alcohol mixing, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C,
After cooling, deionized water washes sodium chloride salt off, can obtain dispersed nano aluminium oxide after being dried.
Embodiment 31
Take 3 grams of the algeldrate hydrosol containing 1.5% weight ratio, weigh 0.9 gram of sodium chloride, add hydrated hydroxide
Change in the aluminum hydrosol, ultrasonic disperse becomes the transparent hydration aluminum hydroxide sol containing sodium chloride.By this algeldrate colloidal sol
Mix with 5 milliliters of dehydrated alcohol, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, little in 750 DEG C of calcinings 1
When, after cooling, deionized water washes sodium chloride salt off, can obtain dispersed nano aluminium oxide after being dried.
Embodiment 32
Take 3 grams of the algeldrate hydrosol containing 1% weight ratio, weigh 0.9 gram of sodium chloride, add hydronium(ion) oxidation
In the aluminum hydrosol, ultrasonic disperse becomes the transparent hydration aluminum hydroxide sol containing sodium chloride.By this algeldrate colloidal sol and 5
Milliliter dehydrated alcohol mixing, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C,
After cooling, deionized water washes sodium chloride salt off, can obtain dispersed nano aluminium oxide after being dried.
Embodiment 33
Take 3 grams of the algeldrate hydrosol containing 30% weight ratio, weigh 0.09 gram of sodium chloride, add hydrated hydroxide
Change in the aluminum hydrosol, ultrasonic disperse becomes the transparent hydration aluminum hydroxide sol containing sodium chloride.By this algeldrate colloidal sol
Mix with 5 milliliters of dehydrated alcohol, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, little in 750 DEG C of calcinings 1
When, after cooling, deionized water washes sodium chloride salt off, can obtain dispersed nano aluminium oxide after being dried.
Embodiment 34
Take 3 grams of the algeldrate hydrosol containing 30% weight ratio, weigh 0.45 gram of sodium chloride, add hydrated hydroxide
Change in the aluminum hydrosol, ultrasonic disperse becomes the transparent hydration aluminum hydroxide sol containing sodium chloride.By this algeldrate colloidal sol
Mix with 5 milliliters of dehydrated alcohol, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, little in 750 DEG C of calcinings 1
When, after cooling, deionized water washes sodium chloride salt off, can obtain dispersed nano aluminium oxide after being dried.
Embodiment 35
Take 3 grams of the algeldrate hydrosol containing 30% weight ratio, weigh 0.72 gram of sodium chloride, add hydrated hydroxide
Change in the aluminum hydrosol, ultrasonic disperse becomes the transparent hydration aluminum hydroxide sol containing sodium chloride.By this algeldrate colloidal sol
Mix with 5 milliliters of dehydrated alcohol, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, little in 750 DEG C of calcinings 1
When, after cooling, deionized water washes sodium chloride salt off, can obtain dispersed nano aluminium oxide after being dried.
Embodiment 36
Take 3 grams of the anatase-type titanium oxide hydrosol containing 10% weight ratio, weigh 0.6 gram of sodium chloride, add anatase
In the type titanium oxide hydrosol, ultrasonic disperse becomes the transparent anatase-type titanium oxide colloidal sol containing sodium chloride.By this Detitanium-ore-type oxygen
Change the titanium hydrosol to mix with 5 milliliters of dehydrated alcohol, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, 750
DEG C calcining 1 hour, after cooling, deionized water washes sodium chloride salt off, can obtain single dispersing rutile type nano titanium oxide after being dried.
Embodiment 37
Take 3 grams of the γ type alumina hydrosol containing 10% weight ratio, weigh 0.6 gram of potassium chloride, add γ type aluminium oxide
In the hydrosol, ultrasonic disperse becomes the transparent γ type alumina sol containing potassium chloride.By this γ type alumina sol and 5 milliliters of nothings
Water-ethanol mixes, and precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 1100 DEG C, after cooling
Deionized water washes potassium chloride salt off, can obtain single dispersing α type nano aluminium oxide after being dried.
Embodiment 38
Take 3 grams of the Yttrium carbonate (Y2(CO3)3) hydrosol containing 10% weight ratio, weigh 0.6 gram of potassium chloride, add in the Yttrium carbonate (Y2(CO3)3) hydrosol,
Ultrasonic disperse becomes the transparent Yttrium carbonate (Y2(CO3)3) colloidal sol containing potassium chloride.This Yttrium carbonate (Y2(CO3)3) colloidal sol is mixed with 5 milliliters of dehydrated alcohol, will precipitate
Thing is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, is dried, and calcines 1 hour at 700 DEG C, after cooling, deionized water washes chlorination off
Potassium salt, can obtain dispersed nano yittrium oxide after being dried.
Embodiment 39
Take 3 grams of the basic magnesium carbonate hydrosol containing 10% weight ratio, weigh 0.6 gram of potassium chloride, add basic magnesium carbonate
In the hydrosol, ultrasonic disperse becomes the transparent basic magnesium carbonate colloidal sol containing potassium chloride.By this basic magnesium carbonate colloidal sol and 5 milliliters of nothings
Water-ethanol mixes, and precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 700 DEG C, after cooling
Deionized water washes potassium chloride salt off, can obtain dispersed nano magnesium oxide after being dried.
Embodiment 40
Take 3 grams of the aluminium carbonate ammonium hydrosol containing 10% weight ratio, weigh 0.6 gram of potassium chloride, add aluminium carbonate ammonium water-soluble
In glue, ultrasonic disperse becomes the transparent aluminium carbonate ammonium colloidal sol containing potassium chloride.This aluminium carbonate ammonium colloidal sol and 5 milliliters of dehydrated alcohol are mixed
Close, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 700 DEG C, after cooling, use deionization
Water-wash away potassium chloride salt, after being dried, dispersed nano aluminium oxide can be obtained.
Embodiment 41
Take 3 grams of the algeldrate hydrosol containing 10% weight ratio, weigh 0.2 gram of potassium sulfate, add hydrated hydroxide
Change in the aluminum hydrosol, ultrasonic disperse becomes the transparent hydration aluminum hydroxide sol containing potassium sulfate.By this algeldrate colloidal sol
Mix with 5 milliliters of dehydrated alcohol, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, little in 1000 DEG C of calcinings 1
When, after cooling, deionized water washes potassium sulfate salt off, can obtain dispersed nano aluminium oxide after being dried.
Embodiment 42
Take 3 grams of the algeldrate hydrosol containing 10% weight ratio, weigh 0.2 gram of potassium sulfate, add hydrated hydroxide
Change in the aluminum hydrosol, ultrasonic disperse becomes the transparent hydration aluminum hydroxide sol containing potassium sulfate.By this algeldrate colloidal sol
Mix with 5 milliliters of dehydrated alcohol, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 0.5 at 1200 DEG C
Hour, after cooling, deionized water washes potassium sulfate salt off, can obtain single dispersing α type nano aluminium oxide after being dried.
Embodiment 43
Take 3 grams of the algeldrate hydrosol containing 10% weight ratio, weigh 0.2 gram of sodium sulfate, add hydrated hydroxide
Change in the aluminum hydrosol, ultrasonic disperse becomes the transparent hydration aluminum hydroxide sol containing sodium sulfate.By this algeldrate colloidal sol
Mix with 5 milliliters of dehydrated alcohol, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, little in 800 DEG C of calcinings 1
When, after cooling, deionized water washes sodium sulfate salt off, can obtain dispersed nano aluminium oxide after being dried.
Embodiment 44
Take 3 grams of the algeldrate hydrosol containing 10% weight ratio, weigh 0.2 gram of sodium sulfate, add hydrated hydroxide
Change in the aluminum hydrosol, ultrasonic disperse becomes the transparent hydration aluminum hydroxide sol containing sodium sulfate.By this algeldrate colloidal sol
Mix with 5 milliliters of dehydrated alcohol, precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 0.5 at 1200 DEG C
Hour, after cooling, deionized water washes sodium sulfate salt off, can obtain single dispersing α type nano aluminium oxide after being dried.
Embodiment 45
Take the γ type containing 10% weight ratio to aoxidize 3 grams of ferrum collosol, weigh 0.6 gram of sodium chloride, add γ type oxidation molten iron
In colloidal sol, ultrasonic disperse becomes the transparent γ type oxidation ferrum collosol containing sodium chloride.By this γ type ferrum oxide hydrosol and 5 milliliters of nothings
Water-ethanol mixes, and precipitate is centrifuged, uses dehydrated alcohol supersound washing 1-2 time, be dried, calcine 1 hour at 750 DEG C, after cooling
Deionized water washes sodium chloride salt off, can obtain α type dispersed nano ferrum oxide after being dried.
Above-described embodiment be only the preferred embodiment of the present invention it should be pointed out that: for the ordinary skill of the art
For personnel, under the premise without departing from the principles of the invention, some improvement and equivalent can also be made, these are to the present invention
Claim improves and the technical scheme after equivalent, each falls within protection scope of the present invention.
Claims (9)
1. a kind of method preparing dispersed nano oxide particle is it is characterised in that the method comprises the following steps:
1) soluble-salt is dissolved in the hydrosol of nano-oxide presoma；
2) the described hydrosol is mixed with weak polar solvent, make soluble-salt with superfine nano graininess separate out, and with nanometer
Oxide precursor granule co-precipitation；
3) by described step 2) centrifugation of the precipitate that obtains, washing, it is dried, calcine below soluble-salt boiling point；
4) deionized water washes the soluble-salt in calcined product off, can obtain dispersed nano oxide particle after being dried.
2. a kind of method preparing dispersed nano oxide particle according to claim 1 is it is characterised in that described receive
Rice oxide precursor is the presoma of following nano-oxide: aluminium oxide, titanium oxide, ferrum oxide, magnesium oxide, zirconium oxide, oxygen
Change copper, nickel oxide, stannum oxide, Indium sesquioxide., yittrium oxide, europium oxide, cerium oxide, lanthana, terbia. Diterbium trioxide, dysprosia or Dineodymium trioxide.
3. a kind of method preparing dispersed nano oxide particle according to claim 1 is it is characterised in that described can
Soluble refers to sodium chloride, potassium chloride, sodium bromide, potassium bromide, sodium sulfate or potassium sulfate.
4. a kind of method preparing dispersed nano oxide particle according to claim 1 is it is characterised in that described receive
Rice oxide precursor is hydrous oxide corresponding to nano-oxide, carbonate, ammonium carbonate salts or subcarbonate, described
Nano-oxide presoma is water insoluble and can decompose generation at high temperature or be converted into nano-oxide.
5. a kind of method preparing dispersed nano oxide particle according to claim 1 is it is characterised in that described receive
Rice oxide precursor is γ type nano aluminium oxide, and described γ type nano aluminium oxide can be converted into α type nanometer more than 1000 DEG C
Aluminium oxide.
6. a kind of method preparing dispersed nano oxide particle according to claim 1 is it is characterised in that described receive
Rice oxide precursor is anatase-type nanometer titanium dioxide, and described anatase-type nanometer titanium dioxide can turn more than 600 DEG C
Turn to rutile titanium dioxide.
7. a kind of method preparing dispersed nano oxide particle according to claim 1 is it is characterised in that described receive
Rice oxide precursor is γ type nano-sized iron oxide, and described γ type nano-sized iron oxide can be converted into α type nano oxygen more than 400 DEG C
Change ferrum.
8. a kind of method preparing dispersed nano oxide particle according to claim 1 is it is characterised in that described water
In colloidal sol, mass ratio >=0.05 of soluble-salt and nano-oxide presoma.
9. a kind of method preparing dispersed nano oxide particle according to claim 1,2,3,4,5,6,7 or 8, its
It is characterised by, described weak polar solvent is acetone, methanol, ethanol, propanol, isopropanol or the tert-butyl alcohol.
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| CN115744993A (en) * | 2022-11-04 | 2023-03-07 | 济南大学 | Large-batch synthesis of ultra-small Mn 3 O 4 Method for preparing nano enzyme |
| CN115744993B (en) * | 2022-11-04 | 2024-06-07 | 济南大学 | Large-scale synthesis of ultra-small Mn3O4Method for preparing nano enzyme |
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