CN105233968B - A kind of method for separating different-grain diameter nano-particle - Google Patents
A kind of method for separating different-grain diameter nano-particle Download PDFInfo
- Publication number
- CN105233968B CN105233968B CN201510338613.0A CN201510338613A CN105233968B CN 105233968 B CN105233968 B CN 105233968B CN 201510338613 A CN201510338613 A CN 201510338613A CN 105233968 B CN105233968 B CN 105233968B
- Authority
- CN
- China
- Prior art keywords
- nano
- separated
- particle
- nanometer powder
- solvent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000002245 particle Substances 0.000 claims abstract description 65
- 239000000843 powder Substances 0.000 claims abstract description 54
- 239000002904 solvent Substances 0.000 claims abstract description 47
- 229910052715 tantalum Inorganic materials 0.000 claims description 44
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 39
- 238000005119 centrifugation Methods 0.000 claims description 22
- 238000000926 separation method Methods 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 18
- 239000006185 dispersion Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 5
- 238000009826 distribution Methods 0.000 abstract description 16
- 241000700605 Viruses Species 0.000 abstract description 2
- 230000009471 action Effects 0.000 abstract description 2
- 238000002955 isolation Methods 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 13
- 235000013339 cereals Nutrition 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000003556 assay Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- BDWFYHUDXIDTIU-UHFFFAOYSA-N ethanol;propane-1,2,3-triol Chemical compound CCO.OCC(O)CO BDWFYHUDXIDTIU-UHFFFAOYSA-N 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- -1 ehter bond Chemical group 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 235000011187 glycerol Nutrition 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000010415 colloidal nanoparticle Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002563 ionic surfactant Substances 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention provides a kind of method for separating different-grain diameter nano-particle, this method is by the way that nanometer powder is well-dispersed in the solvent with specific viscosity, under the centrifugal action of different rotating speeds can the narrow different-grain diameter of isolated particle diameter distribution nano-particle, this method is simple and easy to do, it is simple to operate, the density of solvent in mixed system need not be adjusted, it becomes possible to obtain the narrow nanometer powder of particle diameter distribution, Success rate of virus isolation is high.
Description
Technical field
The present invention relates to a kind of separation method, the method for more particularly to separating different-grain diameter nano-particle.
Background technology
Nano-particle is the minitype particle that a kind of made, size is no more than 100 nanometers.It is probably gel,
Polymer, ceramic particle, metallic particles and carbon particle, it is increasingly being applied in medical science, sun care preparations etc..
Nano-particle has important scientific research value, because it has been set up between bulk matter and atom, molecule
Bridge.The physical property of bulk matter is generally unrelated with size, but but generally really not so on nano-scale.
Nano-particle has special physical effect, thermal property, magnetic performance, optical property etc., as quantum size is imitated
Should, small-size effect, skin effect, macro quanta tunnel effect, coulomb block with quantum tunneling effect, Dielectric confinement effect,
The conventional particle fusing point of nano-particle material more of the same race reduces, starts sintering temperature reduction, crystallization temperature reduces, coercivity is high,
Superparamagnetism, Curie temperature are low, magnetic susceptibility is high, broadband absorbs by force, have blue shift and Red Shift Phenomena, can excite it is luminous etc., because
This, the research to nano-particle at present turns into focus.
The nano-particle of different-grain diameter has a different purposes, and the nano-particle application of narrow particle size distribution is more wide
It is general, the nano-particle using narrow particle size distribution is such as more desirable in computer chip, however, the current nanoparticle that can be obtained
The size distribution of son is wide, and such as between 100nm~1000nm, therefore, be badly in need of solving after nano material synthesis one asks
Topic is how the nano particle of different-grain diameter to separate.
The method of separation oil-soluble nano particles in the prior art be present, as Chinese patent CN101712011A discloses one
Kind of organic density gradient is centrifuged at a high speed the methods of oil-soluble nano particles, and it is molten that colloidal nanoparticles are made in nano-particle by it
Liquid, by hybrid density different organic solvent or Polymer Solution, organic density gradient media is prepared, in centrifuge tube successively
Add various concentrations organic density gradient media, the colloidal solution of nano-particle is added in organic density gradient carry out from
The heart, so as to separate oil-soluble nano particles, this method is when separating the nano-particle of different-grain diameter, it is necessary to constantly adjust organic molten
The density of liquid, and the operation requires very high to the operative skill of operating personnel, easily causes separation to fail.
The method of separation water soluble nanometer particles Selective Separation, such as Chinese patent in the prior art also be present
CN102614975A, discloses a kind of method for water soluble nanometer particles Selective Separation, and this method is selected and treated first
The ionic surfactant of nano-particle oppositely charged has been separated as extractant, then by the method for extraction by aqueous phase
Small size nano-particle is extracted to oil phase and realizes separation.The selectivity of this method is not strong, to the grain of the nano-particle extracted
Footpath can not be expected, surfactant also more difficult selection.
Therefore, it is controllable to need a kind of operating condition of exploitation badly, the separation nanoparticle of the size tunable for the nano-particle isolated
The method of son.
The content of the invention
In order to solve the above problems, present inventor has performed studying with keen determination, as a result find：Nanometer powder is well-dispersed in
, can isolated particle diameter distribution narrow different-grain diameter under the centrifugal action of different rotating speeds in solvent with specific viscosity
Nano-particle, so as to complete the present invention.
It is an object of the invention to provide following aspect：
In a first aspect, the present invention provides a kind of method for separating different-grain diameter nano-particle, it is characterised in that this method bag
Include following steps：
(1) nanometer powder to be separated is scattered in solvent；
(2) dispersion for obtaining step 1 is centrifuged；
(3) remove step 2 and obtain mixture liquid at the middle and upper levels, the precipitum obtained in step 2 is washed, dried；
(4) to the operation of the upper liquid repeat step 2~3 removed in step 3, until nanometer powder to be separated has been separated
Entirely.
Brief description of the drawings
Fig. 1 shows the grain-size graph of nano-tantalum to be separated in embodiment 1；
Fig. 2 shows the grain-size graph of the isolated nano-tantalum under the conditions of rotating speed is 1000rpm in embodiment 1；
Fig. 3 shows the grain-size graph of the isolated nano-tantalum under the conditions of rotating speed is 1500rpm in embodiment 1；
Fig. 4 shows the grain-size graph of the isolated nano-tantalum under the conditions of rotating speed is 2000rpm in embodiment 1；
Fig. 5 shows the grain-size graph of the isolated nano-tantalum under the conditions of rotating speed is 2500rpm in embodiment 1.
Embodiment
Below by the present invention is described in detail, the features and advantages of the invention will become more with these explanations
To be clear, clear and definite.
The present invention described below.
According to the first aspect of the invention, there is provided a kind of method for separating different-grain diameter nano-particle, it is characterised in that institute
The method of stating comprises the following steps：
Step 1, nanometer powder to be separated is scattered in solvent.
In the present invention, nanometer powder to be separated refers to that needs obtain the nanometer powder of narrower particle diameter distribution, such as nano oxygen
Change zinc, nanometer aluminium powder, nano-tantalum etc..
In the present invention, it is preferred to the particle diameter of nanometer powder to be separated is 20nm~400nm, preferably 60nm~310nm；When
When the particle diameter of nanometer powder to be separated is more than 400nm, nanometer powder easily settles in a solvent, and centrifugally operated is to nanometer powder grain
The selectivity in footpath is not high, i.e. most of nano-particle settles down under smaller rotating speed, isolated nano particle diameter
Distribution is wide；When the particle diameter of nanometer powder to be separated is less than 20nm, nanometer powder is very unlikely to settle in solvent, only works as rotating speed
Nano-particle can just settle down when very high, and can not be by nano-particle class settling.
Tantalum has very outstanding chemical property, and its corrosion resistance is high, either under conditions of cold and hot, to salt
Acid, concentrated nitric acid and " chloroazotic acid " do not react, therefore its application field is very extensive.
Therefore, in the present invention, nanometer powder to be separated preferably selects nano-tantalum, more preferably particle diameter be 60nm~
310nm nano-tantalum.
In the present invention, the solvent does not react to each other with nanometer powder to be separated, moreover, the solvent have it is specific
Viscosity, for variety classes and the nanometer powder to be separated of particle diameter, the solvent of different viscositys is selected, makes nanometer powder to be separated
It is suspended in wherein, can be fully dispersed and will not reunites wherein.
In the present invention, when nanometer powder to be separated is the nano-tantalum that particle diameter distribution is 60nm~310nm, selection is glutinous
Spend for 10mPa.s~120mPa.s (16 DEG C), preferably 20mPa.s~70mPa.s (16 DEG C), more preferably 20mPa.s~
40mPa.s (16 DEG C) solvent, in the present invention, the solvent can be the solvent of one-component, or two kinds or more
Double solvents, such as ethylene glycol, Decanol or ethanol-glycerol double solvents obtained by kind solvent complex, nano-tantalum is at it
In good dispersion degree, and be not easy to form reunion, and under appropriate rotating speed, nano-tantalum can obtain that particle diameter distribution is narrower to be received
Rice tantalum particle；When the viscosity of solvent is more than 120mPa.s (16 DEG C), nanometer powder to be separated is reunited seriously, no in a solvent
Energy fine dispersion, so as to which the nano particle diameter distribution obtained after centrifugation is wide；When the viscosity of solvent is less than 10mPa.s
When (16 DEG C), nanometer powder to be separated easily settles in a solvent, it is impossible to forms good suspension, is unfavorable for separating.
The inventors discovered that can be with when hydroxyl, ehter bond, sulphur atom, oxygen atom or nitrogen-atoms etc. on solvent molecule be present
During the functional group of metal-complexing, the decentralization of nano-tantalum wherein greatly improves, and therefore, in the present invention, solvent preferably selects
It is 20mPa.s~120mPa.s (16 DEG C), preferably 20mPa.s~70mPa.s (16 DEG C), more preferably 20mPa.s from viscosity
~40mPa.s (16 DEG C) alcohol compound, preferably ethylene glycol, Decanol or ethanol-glycerol double solvents, such as second two
Alcohol.
The inventors discovered that the viscosity of ethylene glycol is 25.66mPa.s (16 DEG C), and there is the hydroxyl of 2 times of equivalents thereon
Functional group, its peptizaiton to nano-tantalum is strong, and in later separation operating procedure, the nano-tantalum of different-grain diameter is also easy
It is separated, obtains the narrow nanometer tantalum particle of particle diameter distribution, therefore, the present invention preferably ethylene glycol is as solvent.
In the present invention, the amount ratio of nanometer powder and solvent to be separated is the weight of nanometer powder to be separated:Solvent
Volume=(0.1~0.4) parts by weight:50 parts by volume, it is preferably (0.2~0.3) parts by weight:50 parts by volume, wherein, counted based on 1g
For 1 parts by weight, 1 parts by volume is calculated as based on 1mL；When the weight of nanometer powder to be separated:The volume of solvent is more than 0.4 parts by weight:
During 50 parts by volume, nanometer powder to be separated is excessive in solvent, and in separation, the nano-particle of big particle diameter is easily by small particle nanometer
Particle entrainment settles, and causes separation to fail；When the weight of nanometer powder to be separated:The volume of solvent is less than 0.1 parts by weight:50 bodies
During product part, the amount of nanometer powder to be separated is too small in solvent, the step of adding operation, not only wastes solvent, and add
Time and financial cost.
In the present invention, the dispersing mode of nanometer powder to be separated in a solvent is not specially limited, so as to be separated
It is preferred, such as magnetic agitation, mechanical agitation, sonic oscillation, preferably sonic oscillation that nanometer powder is fully dispersed in a solvent.
Step 2, dispersion step 1 obtained is centrifuged.
The dispersion that step 1 obtains is centrifuged for the first time under smaller rotating speed, wherein the larger nanometer of particle diameter
Particle precipitation comes out.
It is not bound by any theory, inventors believe that, when centrifuge is run, material is subject in centrifuge centrifugal force
Much larger than the gravity that it is subject to, therefore, in centrifugal separation processes, it is heavy that the nanometer powder in the dispersion that step 1 obtains has
The trend of drop, and its centrifugal force for being subject to of the nano-particle of different-grain diameter is different, its in the presence of same angular velocity, particle diameter compared with
Big nano-particle is settled first, and the less nano-particle of particle diameter is still suspended in mixed system, though increase from
Heart time, the less nano-particle of particle diameter will not also settle.
In the present invention, when separating the nano-particle of different-grain diameter, the rotating speed of centrifugation is that can make current mixed system
The minimum speed of middle nano-particle sedimentation, centrifugation time are that the nano-particle for allowing to sedimentation is fully settled into preferably.
In one preferred embodiment of the invention, when nanometer powder to be separated is that particle diameter is receiving for 60nm~310nm
Rice tantalum powder, when solvent for use is ethylene glycol, preferably nano-tantalum and ethylene glycol are according to the weight that w/v is nano-tantalum:
Volume=0.2639g of ethylene glycol:50mL, which carries out mixing, to be disperseed, and rotating speed when centrifuging first is 800~1200rpm, excellent
Elect 1000rpm as, centrifugation time is 20~40min, preferably 30min.
The inventors discovered that when the rotating speed centrifuged first is 800~1200rpm, preferably 1000rpm, you can
Obtain the nano-particle of the narrower greater particle size of particle diameter distribution.
Step 3, remove step 2 and obtain mixture liquid at the middle and upper levels, the precipitum obtained in step 2 is washed, dried.
Step 2 obtains mixture, and liquid is still nanometer powder and the mixed system of solvent at the middle and upper levels, is moved out separation system
Treat further to separate.
The precipitum that step 2 is obtained is washed, and the present invention is not specially limited to washing methods, that will can obtain
The impurity of precipitum adsorption to remove be preferred, such as washed with ethanol, then filter removing cleaning solution etc..
In the present invention, drying mode is not specially limited, can be dried using any one solid in the prior art
Mode, such as constant-pressure and high-temperature are dry, decompression high temperature drying, are preferably dried in vacuo.
In the present invention, drying time is not specially limited, that can be preferred by products therefrom fully drying.
In one preferred embodiment of the invention, the precipitum that step 2 obtains is washed 3 times with absolute ethyl alcohol, then
Obtained product is dried in vacuo 1 hour at 40 DEG C.
Step 4, to the operation of the upper solution repeat step 2~3 removed in step 3, until nanometer powder quilt to be separated
Separation is complete.
The upper liquid removed in step 3 is repeated the above steps 2~3 operation, difference is to adjust different centrifugation speed
Degree.
The inventors discovered that when nanometer powder is centrifuged, rotating speed is incremented by 300~800rpm every time, preferably
For 500rpm, the narrow nanoparticle mixture of particle diameter distribution can be obtained.
In the preferred embodiment of the present invention, when nanometer powder to be separated is that particle diameter is 60nm~310nm's
Nano-tantalum, solvent for use are ethylene glycol, preferably weight of the nano-tantalum with ethylene glycol according to w/v for nano-tantalum:
Volume=0.2639g of ethylene glycol:50mL, which carries out mixing, to be disperseed, and rotating speed when centrifuging first is 800~1200rpm, excellent
Elect 1000rpm as, centrifugation time is 20~40min, and preferably 30min is carried out after separating first, selected when separating for second from
The rotating speed of heart separation is 1300~1700rpm, preferably 1500rpm, and centrifugation time is 20~40min, preferably 30min；The
The rotating speed that selection centrifuges when separating three times be 1800~2200rpm, preferably 2000rpm, centrifugation time for 20~
40min, preferably 30min；The rotating speed that selection centrifuges during the 4th separation is 2300~2700rpm, is preferably
2500rpm, centrifugation time are 20~40min, preferably 30min.
The inventors discovered that in above-mentioned preferred embodiment, by four centrifugations, you can tantalum powder is separated into
Particle diameter is respectively 240.7~303.6nm, 164.9~252.3nm, 135.7~171.2nm and 71.4~90.1nm particle diameter point
The narrow tantalum powder powder of cloth.
According to different-grain diameter nano-particle separation method provided by the invention, have the advantages that：
(1) the narrow nanometer powder of particle diameter distribution can be obtained using method provided by the invention；
(2) provided by the invention method is simple, simple to operate, it is not necessary to the density of solvent in mixed system is adjusted,
Success rate of virus isolation is high；
(3) equipment that this method uses is conventional, and cost is cheap；
(4) solvent used in this method is green, and environmental pollution is small；
(5) post processing of this method to isolated nano-powder is easy, easily operated.
Embodiment
(1) measure of particle diameter of nanometer powder
The particle diameter of nano-powder is measured using laser particle size method in the present invention.
Embodiment 1
(1) by the nano-tantalum of 0.2639g (assay balance weighing) (with the method for (one) determine its particle diameter for 61.1~
306.6nm, its grain-size graph are as shown in Figure 1) it is scattered in 50mL ethylene glycol, fully dispersed 30 minutes in ultrasonic machine, then it will divide
The mixed liquor dissipated is loaded in centrifuge tube；
(2) centrifuged 30 minutes under conditions of rotating speed is 1000rpm；
(3) upper liquid is removed into separation system, the precipitum that centrifugation obtains washed 3 times with absolute ethyl alcohol, at 40 DEG C
Vacuum drying 1 hour, after ultrasonic disperse in absolute ethyl alcohol, the particle diameter of precipitum is determined with the method for (one), its particle diameter is
240.7~303.6nm, grain-size graph are as shown in Figure 2；
(4) upper liquid continues to be centrifuged under conditions of rotating speed is 1500rpm, 2000rpm and 2500rpm respectively
30min, the operation of previous step 2~3 is repeated, untill upper liquid is clarified, that is, the minimum grain size for the powder for settling to obtain is
Untill the minimum grain size of nanometer powder to be separated.
The particle diameter for the nano-tantalum for centrifuging to obtain in the case where rotating speed is 1500rpm is 164.9nm~252.3nm, and grain-size graph is such as
Shown in Fig. 3.
The particle diameter for the nano-tantalum for centrifuging to obtain in the case where rotating speed is 2000rpm is 135.7nm~171.2nm, and grain-size graph is such as
Shown in Fig. 4.
The particle diameter for the nano-tantalum for centrifuging to obtain in the case where rotating speed is 2500rpm is 71.4nm~90.1nm, grain-size graph such as Fig. 5
It is shown.
From embodiment 1, nano-tantalum can be scattered in ethylene glycol, in 1000rpm, 1500rpm, 2000rpm and
30min is centrifuged to dispersion successively under conditions of 2500rpm, 4 kinds of different-grain diameter grades can be obtained and particle diameter distribution is narrow
Nano-tantalum, moreover, with the increase of rotating speed, the particle diameter of obtained nano-tantalum is smaller.
Embodiment 2
(1) by the nano-tantalum of 0.3998g (assay balance weighing) (with the method for (one) determine its particle diameter for 60.1~
310.6nm) be scattered in 50mL Decanols, fully dispersed 30 minutes in ultrasonic machine, then by scattered mixed liquor be loaded on from
In heart pipe；
(2) centrifuged 40 minutes under conditions of rotating speed is 800rpm；
(3) upper liquid is removed into separation system, the precipitum that centrifugation obtains washed 3 times with absolute ethyl alcohol, at 40 DEG C
Vacuum drying 1 hour, after ultrasonic disperse in absolute ethyl alcohol, the particle diameter of precipitum is determined with the method for (one), its particle diameter is
250~310nm；
(4) upper liquid continues to be centrifuged under conditions of rotating speed is 1300rpm, 1800rpm and 2300rpm respectively
40min, the operation of previous step 2~3 is repeated, untill upper liquid is clarified, that is, the minimum grain size for the powder for settling to obtain is
Untill the minimum grain size of nanometer powder to be separated.
The particle diameter for the nano-tantalum for centrifuging to obtain in the case where rotating speed is 1300rpm is 180~240nm.
The particle diameter for the nano-tantalum for centrifuging to obtain in the case where rotating speed is 1800rpm is 100~180nm.
The particle diameter for the nano-tantalum for centrifuging to obtain in the case where rotating speed is 2300rpm is 60~80nm.
Embodiment 3
(1) by the nano-tantalum of 0.1325g (assay balance weighing) (with the method for (one) determine its particle diameter for 20.5~
400.3nm) it is scattered in 50mL ethanol-glycerol double solvents (viscosity 100mPa.S), fully dispersed 30 in ultrasonic machine
Minute, then scattered mixed liquor is loaded in centrifuge tube；
(2) centrifuged 20 minutes under conditions of rotating speed is 1200rpm；
(3) upper liquid is removed into separation system, the precipitum that centrifugation obtains washed 3 times with absolute ethyl alcohol, at 40 DEG C
Vacuum drying 1 hour, after ultrasonic disperse in absolute ethyl alcohol, the particle diameter of precipitum is determined with the method for (one), its particle diameter is
150~200nm；
(4) upper liquid continues to be centrifuged under conditions of rotating speed is 1700rpm, 2200rpm and 2700rpm respectively
20min, the operation of previous step 2~3 is repeated, untill upper liquid is clarified, that is, the minimum grain size for the powder for settling to obtain is
Untill the minimum grain size of nanometer powder to be separated.
The particle diameter for the nano-tantalum for centrifuging to obtain in the case where rotating speed is 1700rpm is 100~120nm.
The particle diameter for the nano-tantalum for centrifuging to obtain in the case where rotating speed is 2200rpm is 50~80nm.
The particle diameter for the nano-tantalum for centrifuging to obtain in the case where rotating speed is 2700rpm is 20~30nm.
Comparative example 1
This comparative example method therefor is similar to Example 1, and the particle diameter for differing only in nano-tantalum used is 1~20nm,
As a result nano-tantalum can not be separated.
Comparative example 2
This comparative example method therefor is similar to Example 2, differ only in the particle diameter of nano-tantalum used for 400~
600nm, it as a result can not separate nano-tantalum.
Comparative example 3
This comparative example method therefor is similar to Example 3, and it is that (viscosity is absolute ethyl alcohol to differ only in solvent for use
1.2mPa.S), as a result nano-tantalum can not disperse to form suspension in absolute ethyl alcohol, but all settle.
Comparative example 4
This comparative example method therefor is similar to Example 3, and it is that (viscosity is glycerine to differ only in solvent for use
1163mPa.S), as a result nano-tantalum can not reunite in glycerine, and rotating speed when increase centrifuges, tantalum powder can not also settle.
The present invention is described in detail above in association with embodiment and exemplary example, but these explanations are simultaneously
It is not considered as limiting the invention.It will be appreciated by those skilled in the art that without departing from the spirit and scope of the invention,
A variety of equivalencing, modification or improvement can be carried out to technical solution of the present invention and embodiments thereof, these each fall within the present invention
In the range of.Protection scope of the present invention is determined by the appended claims.
Claims (5)
- A kind of 1. method for separating different-grain diameter nano-particle, it is characterised in that this method comprises the following steps：（1）Nanometer powder to be separated is scattered in solvent, the particle diameter of the nanometer powder to be separated is 20nm ~ 400nm, described Nanometer powder to be separated is nano-tantalum, and the solvent is ethylene glycol,The amount ratio of nanometer powder and solvent to be separated is the weight of nanometer powder to be separated:The volume of solvent=（0.1~0.4）Weight Measure part:50 parts by volume, wherein, 1 parts by weight are calculated as based on 1g, 1 parts by volume is calculated as based on 1mL；（2）The dispersion that step 1 is obtained is centrifuged, and the rotating speed centrifuged first is 800 ~ 1200rpm, centrifugation time For 20 ~ 40min；（3）Remove step 2 and obtain mixture liquid at the middle and upper levels, the precipitum obtained in step 2 is washed, dried；（4）To the operation of the upper liquid repeat step 2 ~ 3 removed in step 3, until nanometer powder to be separated is separated completely,Second of rotating speed for selecting to centrifuge when separating is 1300 ~ 1700rpm, and centrifugation time is 20 ~ 40min；The rotating speed that selection centrifuges when third time separates is 1800 ~ 2200rpm, and centrifugation time is 20 ~ 40min；WithThe rotating speed that selection centrifuges during the 4th separation is 2300 ~ 2700rpm, and centrifugation time is 20 ~ 40min.
- 2. according to the method for claim 1, it is characterised in that in step 1, the particle diameter of the nanometer powder to be separated is 60nm~310nm。
- 3. according to the method for claim 1, it is characterised in that in step 1, the dosage of nanometer powder and solvent to be separated Than the weight for nanometer powder to be separated:The volume of solvent=（0.2~0.3）Parts by weight:50 parts by volume, wherein,1 parts by weight are calculated as based on 1g, 1 parts by volume is calculated as based on 1mL.
- 4. according to the method for claim 1, it is characterised in that in step 2, the rotating speed of centrifugation is 1000rpm, during centrifugation Between be 30min.
- 5. according to the method for claim 1, it is characterised in that in step 4,Second of rotating speed for selecting to centrifuge when separating is 1500rpm, centrifugation time 30min；The rotating speed that selection centrifuges when third time separates is 2000rpm, centrifugation time 30min；WithThe rotating speed that selection centrifuges during the 4th separation is 2500rpm, centrifugation time 30min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510338613.0A CN105233968B (en) | 2015-06-17 | 2015-06-17 | A kind of method for separating different-grain diameter nano-particle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510338613.0A CN105233968B (en) | 2015-06-17 | 2015-06-17 | A kind of method for separating different-grain diameter nano-particle |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105233968A CN105233968A (en) | 2016-01-13 |
| CN105233968B true CN105233968B (en) | 2017-11-14 |
Family
ID=55031933
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510338613.0A Active CN105233968B (en) | 2015-06-17 | 2015-06-17 | A kind of method for separating different-grain diameter nano-particle |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105233968B (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621354B (en) * | 2016-01-22 | 2019-01-18 | 京东方科技集团股份有限公司 | The partial size thinning method of nano particle and the system refined for nano particle diameter |
| CN106040589B (en) * | 2016-07-11 | 2018-08-31 | 阜阳师范学院 | A method of separation different-grain diameter nanometer aluminium powder |
| CN106607180B (en) * | 2016-12-30 | 2019-02-22 | 广东工业大学 | A kind of separation method of nano particle |
| CN112238001A (en) * | 2019-07-17 | 2021-01-19 | 阜阳师范大学 | Method for differential separation of nano aluminum powder with different particle sizes |
| CN112238002A (en) * | 2019-07-17 | 2021-01-19 | 阜阳师范大学 | Method for differential separation of nano copper powder with different particle sizes |
| CN110586930B (en) * | 2019-10-22 | 2022-01-14 | 广东银纳科技有限公司 | Preparation method of nano titanium material for corrosion prevention |
| CN112452528B (en) * | 2020-11-05 | 2022-04-22 | 苏州易奥秘光电科技有限公司 | Magnetic nanoparticle consistency screening method |
| CN114749656A (en) * | 2020-12-28 | 2022-07-15 | 航天神舟生物科技集团有限公司 | Preparation method of metal nano iron/nano copper particle solution and working solution |
| CN114192770B (en) * | 2021-11-19 | 2024-05-24 | 苏州大学 | Silver colloid and preparation method thereof |
| CN115040903A (en) * | 2022-07-19 | 2022-09-13 | 道生天合材料科技(上海)股份有限公司 | Method for separating filler |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1947848A (en) * | 2006-01-09 | 2007-04-18 | 复旦大学 | Functional magnetic separating rod and its making method |
| CN101185913A (en) * | 2007-09-22 | 2008-05-28 | 兰州大学 | Method for separating metallicity and semiconductivity nano-tube from single wall carbon nano-tube |
| CN101712011A (en) * | 2009-11-13 | 2010-05-26 | 北京化工大学 | Method for centrifugally separating oil soluble nano particles by organic density gradient |
| JP4738611B2 (en) * | 2001-03-12 | 2011-08-03 | 和幸 田路 | Carbon nanotube purification method |
| CN102408228A (en) * | 2011-08-19 | 2012-04-11 | 北京航空航天大学 | Preparation method of synthetic series monodisperse rare earth-doped cobalt ferrite nanoparticle |
-
2015
- 2015-06-17 CN CN201510338613.0A patent/CN105233968B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4738611B2 (en) * | 2001-03-12 | 2011-08-03 | 和幸 田路 | Carbon nanotube purification method |
| CN1947848A (en) * | 2006-01-09 | 2007-04-18 | 复旦大学 | Functional magnetic separating rod and its making method |
| CN101185913A (en) * | 2007-09-22 | 2008-05-28 | 兰州大学 | Method for separating metallicity and semiconductivity nano-tube from single wall carbon nano-tube |
| CN101712011A (en) * | 2009-11-13 | 2010-05-26 | 北京化工大学 | Method for centrifugally separating oil soluble nano particles by organic density gradient |
| CN102408228A (en) * | 2011-08-19 | 2012-04-11 | 北京航空航天大学 | Preparation method of synthetic series monodisperse rare earth-doped cobalt ferrite nanoparticle |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105233968A (en) | 2016-01-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105233968B (en) | A kind of method for separating different-grain diameter nano-particle | |
| JP6209032B2 (en) | Classified particle material, method for producing the same, and resin composition | |
| CN110846028B (en) | Polymer-coated perovskite quantum dot, preparation method thereof and semiconductor luminescent material comprising same | |
| CN105189617B (en) | Optimization emulsion drying means for preparing micronizing polyetherimide polymer | |
| JP5384643B2 (en) | Liquid suspensions and powders of cerium oxide particles, methods for their production and their use in polishing | |
| CN101559401A (en) | Method for separating nano-particles at water-phase density gradient centrifugation rate | |
| CN110296973B (en) | SiO2@ Ag @ ZrO2 multilayer core-shell structure nano material and preparation method and application thereof | |
| JP5446703B2 (en) | Method for producing purified graphite oxide particle-containing liquid | |
| US11707700B2 (en) | Process for interfacial separation of metal nanoparticles or nanowires using centrifugal separators | |
| CN112657475A (en) | Boron affinity functionalized microsphere adsorbent and preparation method and application thereof | |
| Deshpande et al. | Continuous interfacial centrifugal separation and recovery of silver nanoparticles | |
| CN109096499B (en) | Superparamagnetic nano magnetic bead, preparation method thereof and application of controllable emulsification/demulsification performance | |
| CN111233083B (en) | Method for accelerating adsorption and separation of oil-soluble substances by using magnetic Janus emulsion | |
| CN114058353A (en) | Janus modified molybdenum disulfide nano-particles, preparation method thereof and oil displacement material | |
| JP6179015B2 (en) | Granules, method for producing the same, and property modifying material | |
| Costo et al. | Size sorting of ultrasmall magnetic nanoparticles and their aggregates behaviour | |
| CN110026298A (en) | A kind of micro-nano powder partial size centrifugal classification apparatus and its application method | |
| CN106040589A (en) | Method for separating nanometer aluminum powder with different particle sizes | |
| CN108793122A (en) | Preparation method of novel C70 fullerene crystal | |
| CN104138795B (en) | A kind of separation method of different size alpha-aluminium oxide nano-particle | |
| CN107866561A (en) | Extract solution from aloe separation single size In4The method of Ni nanospheres | |
| JP5617992B2 (en) | Method for producing purified graphite oxide particle-containing liquid | |
| CN113860310B (en) | Method for extracting nanoscale silicon carbide from superfine silicon carbide tailings | |
| CN114590807A (en) | Preparation method of nano-diamond dispersed aqueous solution with small particle size | |
| CN103480323A (en) | Method for realizing one-step synthesis of ferroferric oxide microspheres having hierarchical structure and application method of product thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201221 Address after: 465450 in vein Industrial Park, south of 312 National Road, Zhaihe Town, Guangshan County, Xinyang City, Henan Province Patentee after: Henan Soton New Material Co.,Ltd. Address before: 236041 no.741, Qinghe East Road, Fuyang City, Anhui Province Patentee before: Tao Dongliang |
|
| TR01 | Transfer of patent right | ||
| CP02 | Change in the address of a patent holder |
Address after: 453499 No. 3, Pubei pilot industrial park, Changheng County, Xinxiang, Henan Province Patentee after: Henan Soton New Material Co.,Ltd. Address before: 465450 in vein Industrial Park, south of 312 National Road, Zhaihe Town, Guangshan County, Xinyang City, Henan Province Patentee before: Henan Soton New Material Co.,Ltd. |
|
| CP02 | Change in the address of a patent holder | ||
| CP02 | Change in the address of a patent holder |
Address after: 453499 No. 3, Pubei pilot industrial park, Changyuan City, Xinxiang City, Henan Province Patentee after: Henan Soton New Material Co.,Ltd. Address before: 453499 No. 3, Pubei pilot industrial park, Changheng County, Xinxiang, Henan Province Patentee before: Henan Soton New Material Co.,Ltd. |
|
| CP02 | Change in the address of a patent holder |