CN105233968A - Method for separating nano particles of different particle sizes - Google Patents
Method for separating nano particles of different particle sizes Download PDFInfo
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- -1 ehter bond Chemical group 0.000 claims description 3
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Abstract
The invention provides a method for separating nano particles of different particle sizes. According to the method, nano powder is fully dispersed into solvent of certain viscosity, and the nano particles which are of different particle sizes and are narrow in particle size distribution range can be obtained under the centrifugal effect at different rotation speeds. The method is convenient and easy to implement, the operation is easy, the nano powder which is narrow in particle size distribution range can be obtained without adjusting the density of the solvent in a mixed system, and the success rate of separation is high.
Description
Technical field
The present invention relates to a kind of separation method, be particularly separated the method for different-grain diameter nano particle.
Background technology
Nano particle is a kind of made, minitype particle that size is no more than 100 nanometers.It may be gel, polymer, ceramic particle, metallic particles and carbon granule, and it is applied in medical science, sun care preparations etc. more and more.
Nano particle has important scientific research value, because it has set up the bridge between bulk matter and atom, molecule.The physical property of bulk matter is usual and size is irrelevant, but but usually really not so on nano-scale.
Nano particle has special physical effect, thermal property, magnetic performance, optical property etc., as quantum size effect, small-size effect, skin effect, macro quanta tunnel effect, coulomb blocking and quantum tunneling effect, Dielectric confinement effect, the conventional particle fusing point of nano particle material more of the same race reduces, start sintering temperature to reduce, crystallization temperature reduces, coercivity is high, superparamagnetism, Curie temperature is low, magnetic susceptibility is high, broadband absorbs by force, there is blue shift and Red Shift Phenomena, can stimulated luminescence etc., therefore, at present focus is become to the research of nano particle.
The nano particle of different-grain diameter has different purposes, the nano particle range of application of narrow particle size distribution is more extensive, the nano particle of narrow particle size distribution is used as more wished in computer chip, but, the size distribution of the current nano particle that can obtain is wide, as between 100nm ~ 1000nm, therefore, how the nano particle of different-grain diameter separately the problem being badly in need of solving after nano material synthesis is exactly.
The method being separated oil-soluble nano particles is there is in prior art, as Chinese patent CN101712011A discloses a kind of method that organic density gradient high speed centrifugation is separated oil-soluble nano particles, nano particle is made colloidal nanoparticles solution by it, the organic solvent different by hybrid density or Polymer Solution, preparation organic density gradient media, the organic density gradient media of variable concentrations is added successively in centrifuge tube, the colloidal solution of nano particle is added to organic density gradient is carried out centrifugal, thus separation oil-soluble nano particles, the method is when being separated the nano particle of different-grain diameter, need the density of constantly adjustment organic solution, and this operation requires very high to the operative skill of operating personnel, very easily cause being separated unsuccessfully.
The method of separating water-soluble nano particle Selective Separation is also there is in prior art, as Chinese patent CN102614975A, disclose a kind of method for water soluble nanometer particles Selective Separation, first the method is selected with the ionic surfactant of nano particle oppositely charged to be separated as extractant, then by the method for extraction, aqueous phase small-medium size nano particle is extracted to oil phase and realizes being separated.This method selective strong, cannot expect to the particle diameter of the nano particle extracted, surfactant is more difficult selection also.
Therefore, a kind of operating condition of exploitation is needed badly controlled, the method for the separation nano particle of the size tunable of isolated nano particle.
Summary of the invention
In order to solve the problem, present inventor has performed and study with keen determination, found that: nanometer powder is well-dispersed in the solvent with specific viscosity, be the separable nano particle obtaining the different-grain diameter of narrow diameter distribution under the centrifugal action of different rotating speeds, thus complete the present invention.
The object of the present invention is to provide following aspect:
First aspect, the invention provides a kind of method being separated different-grain diameter nano particle, it is characterized in that, the method comprises the following steps:
(1) nanometer powder to be separated is scattered in solvent;
(2) dispersion step 1 obtained carries out centrifugation;
(3) shift out step 2 and obtain mixture liquid at the middle and upper levels, the precipitum obtained in step 2 is washed, dry;
(4) upper liquid shifted out in step 3 is repeated to the operation of step 2 ~ 3, until nanometer powder to be separated is completely separated.
Accompanying drawing explanation
Fig. 1 illustrates the grain-size graph of nano-tantalum to be separated in embodiment 1;
Fig. 2 illustrates the grain-size graph being separated under rotating speed is 1000rpm condition in embodiment 1 and obtaining nano-tantalum;
Fig. 3 illustrates the grain-size graph being separated under rotating speed is 1500rpm condition in embodiment 1 and obtaining nano-tantalum;
Fig. 4 illustrates the grain-size graph being separated under rotating speed is 2000rpm condition in embodiment 1 and obtaining nano-tantalum;
Fig. 5 illustrates the grain-size graph being separated under rotating speed is 2500rpm condition in embodiment 1 and obtaining nano-tantalum.
Detailed description of the invention
Below by the present invention is described in detail, the features and advantages of the invention will illustrate along with these and become more clear, clear and definite.
Below in detail the present invention is described in detail.
According to a first aspect of the invention, a kind of method being separated different-grain diameter nano particle is provided, it is characterized in that, said method comprising the steps of:
Step 1, is scattered in nanometer powder to be separated in solvent.
In the present invention, nanometer powder to be separated refers to the nanometer powder needing to obtain narrower domain size distribution, as nano zine oxide, nanometer aluminium powder, nano-tantalum etc.
In the present invention, the particle diameter of preferred nanometer powder to be separated is 20nm ~ 400nm, is preferably 60nm ~ 310nm; When the particle diameter of nanometer powder to be separated is greater than 400nm, nanometer powder is very easily sedimentation in a solvent, selective not high to nanometer powder particle diameter of centrifugally operated, namely, under less rotating speed, most of nano particle all settles down, and is separated the nano particle diameter distribution obtained wide; When the particle diameter of nanometer powder to be separated is less than 20nm, nanometer powder is not easy sedimentation in solvent pole, only has the nano particle when rotating speed is very high just can settle down, and can not by nano particle class settling.
Tantalum has very outstanding chemical property, and its corrosion resistance is high, no matter is under the condition of cold-peace heat, and do not react hydrochloric acid, red fuming nitric acid (RFNA) and " chloroazotic acid ", therefore its application widely.
Therefore, in the present invention, nanometer powder to be separated preferably selects nano-tantalum, is more preferably the nano-tantalum that particle diameter is 60nm ~ 310nm.
In the present invention, described solvent does not react to each other with nanometer powder to be separated, and, described solvent has specific viscosity, for the nanometer powder to be separated of variety classes and particle diameter, select the solvent of different viscosity, make nanometer powder to be separated be suspended in wherein, fully can disperse and can not reunite wherein.
In the present invention, when nanometer powder to be separated be domain size distribution is the nano-tantalum of 60nm ~ 310nm, selection viscosity is 10mPa.s ~ 120mPa.s (16 DEG C), be preferably 20mPa.s ~ 70mPa.s (16 DEG C), be more preferably the solvent of 20mPa.s ~ 40mPa.s (16 DEG C), in the present invention, described solvent can be the solvent of one-component, the double solvents that also can obtain for two or more solvent complexes, as ethylene glycol, Decanol or ethanol-glycerol double solvents etc., nano-tantalum good dispersion degree wherein, and not easily form reunion, and under suitable rotating speed, nano-tantalum can obtain the narrower nanometer tantalum particle of domain size distribution, when the viscosity of solvent is greater than 120mPa.s (16 DEG C), nanometer powder to be separated is reunited seriously in a solvent, can not fine dispersion, thus the nano particle diameter obtained after centrifugation distribution is wide, when the viscosity of solvent is less than 10mPa.s (16 DEG C), nanometer powder to be separated is very easily sedimentation in a solvent, can not form good suspension, is unfavorable for being separated.
The present inventor finds, when solvent molecule exists hydroxyl, ehter bond, sulphur atom, oxygen atom or nitrogen-atoms etc. can functional group with metal-complexing time, nano-tantalum decentralization wherein improves greatly, therefore, in the present invention, it is 20mPa.s ~ 120mPa.s (16 DEG C) that solvent is preferably selected from viscosity, be preferably 20mPa.s ~ 70mPa.s (16 DEG C), be more preferably the alcohol compound of 20mPa.s ~ 40mPa.s (16 DEG C), be preferably ethylene glycol, Decanol or ethanol-glycerol double solvents, as ethylene glycol.
The present inventor finds, the viscosity of ethylene glycol is 25.66mPa.s (16 DEG C), and it has the hydroxy functional group of 2 times of equivalents, it is strong to the peptizaiton of nano-tantalum, in later separation operating procedure, the nano-tantalum of different-grain diameter is also easily separated to be opened, and obtains the nanometer tantalum particle of narrow diameter distribution, therefore, the preferred ethylene glycol of the present invention is as solvent.
In the present invention, the amount ratio of nanometer powder to be separated and solvent is the weight of nanometer powder to be separated: volume=(0.1 ~ 0.4) weight portion of solvent: 50 parts by volume, be preferably (0.2 ~ 0.3) weight portion: 50 parts by volume, wherein, count 1 weight portion based on 1g, count 1 parts by volume based on 1mL; Weight when nanometer powder to be separated: the volume of solvent is greater than 0.4 weight portion: during 50 parts by volume, in solvent, nanometer powder to be separated is too much, and when being separated, the nano particle of Large stone easily carries small particle diameter nano particle secretly sedimentation, causes and is separated unsuccessfully; Weight when nanometer powder to be separated: the volume of solvent is less than 0.1 weight portion: during 50 parts by volume, and in solvent, the amount of nanometer powder to be separated is too small, adds the step of operation, not only wastes solvent, and adds time and financial cost.
In the present invention, nanometer powder to be separated dispersing mode is not in a solvent particularly limited to, to make nanometer powder to be separated fully be separated into preferably in a solvent, as magnetic agitation, mechanical agitation, sonic oscillation etc., is preferably sonic oscillation.
Step 2, dispersion step 1 obtained carries out centrifugation.
Dispersion step 1 obtained carries out first centrifugation under less rotating speed, and the nano particle that wherein particle diameter is larger settles.
Be not bound by any theory, the present inventor thinks, when centrifuge runs, the gravity that the centrifugal force that in centrifuge, material is subject to is subject to much larger than it, therefore, in centrifugal separation processes, nanometer powder in the dispersion that step 1 obtains has the trend of sedimentation, and its centrifugal force be subject to of the nano particle of different-grain diameter is different, it is under the effect of same angular velocity, and first the nano particle that particle diameter is larger settles, and the less nano particle of particle diameter is still suspended in mixed system, even if increase centrifugation time, the nano particle that particle diameter is less also can not sedimentation.
In the present invention, when being separated the nano particle of different-grain diameter, centrifugal rotating speed is the minimum speed that can make nano particle sedimentation in current mixed system, and centrifugation time is the abundant sedimentation of nano particle allowing to sedimentation is preferred.
In the present invention one preferred embodiment, when the nano-tantalum of nanometer powder to be separated to be particle diameter be 60nm ~ 310nm, when solvent for use is ethylene glycol, preferred nano-tantalum and ethylene glycol are the weight of nano-tantalum according to w/v: the volume=0.2639g:50mL of ethylene glycol carries out mixing and disperses, rotating speed first during centrifugation is 800 ~ 1200rpm, be preferably 1000rpm, centrifugation time is 20 ~ 40min, is preferably 30min.
The present inventor finds, when the rotating speed of centrifugation is first 800 ~ 1200rpm, when being preferably 1000rpm, can obtain the nano particle of the narrower greater particle size of domain size distribution.
Step 3, shifts out step 2 and obtains mixture liquid at the middle and upper levels, wash the precipitum obtained in step 2, dry.
Step 2 obtain mixture at the middle and upper levels liquid be still the mixed system of nanometer powder and solvent, shifted out separation system and treated further separation.
Precipitum step 2 obtained washs, and the present invention is not particularly limited to washing methods, being preferred by the Impurity removal of the precipitum adsorption obtained, as washed with ethanol, then suction filtration removing cleaning solution etc.
In the present invention, drying mode is not particularly limited to, any one solid drying mode in prior art can be used, as constant-pressure and high-temperature drying, decompression high temperature drying etc., be preferably vacuum drying.
In the present invention, drying time is not particularly limited to, with can by products therefrom fully drying be preferred.
In the present invention one preferred embodiment, the precipitum absolute ethanol washing that step 2 is obtained 3 times, then by the vacuum drying 1 hour at 40 DEG C of the product that obtains.
Step 4, repeats the operation of step 2 ~ 3, until nanometer powder to be separated is completely separated to the upper solution shifted out in step 3.
The upper liquid shifted out in step 3 is repeated to the operation of above-mentioned steps 2 ~ 3, difference is to adjust different centrifugal speeds.
The present inventor finds, when carrying out centrifugation to nanometer powder, rotating speed increases progressively 300 ~ 800rpm at every turn, is preferably 500rpm, can obtains the nanoparticle mixture of narrow diameter distribution.
Of the present invention one preferred embodiment in, when the nano-tantalum of nanometer powder to be separated to be particle diameter be 60nm ~ 310nm, solvent for use is ethylene glycol, preferred nano-tantalum and ethylene glycol are the weight of nano-tantalum according to w/v: the volume=0.2639g:50mL of ethylene glycol carries out mixing and disperses, rotating speed first during centrifugation is 800 ~ 1200rpm, be preferably 1000rpm, centrifugation time is 20 ~ 40min, after preferably 30min is separated first, the rotating speed selecting centrifugation when second time is separated is 1300 ~ 1700rpm, be preferably 1500rpm, centrifugation time is 20 ~ 40min, be preferably 30min, the rotating speed selecting centrifugation when third time is separated is 1800 ~ 2200rpm, and be preferably 2000rpm, centrifugation time is 20 ~ 40min, is preferably 30min, the rotating speed selecting centrifugation when being separated for the 4th time is 2300 ~ 2700rpm, and be preferably 2500rpm, centrifugation time is 20 ~ 40min, is preferably 30min.
The present inventor finds, above-mentioned preferred embodiment in, through four centrifugations, tantalum powder can be separated into the tantalum powder powder that particle diameter is respectively the narrow diameter distribution of 240.7 ~ 303.6nm, 164.9 ~ 252.3nm, 135.7 ~ 171.2nm and 71.4 ~ 90.1nm.
According to different-grain diameter nano particle separation method provided by the invention, there is following beneficial effect:
(1) method provided by the invention is utilized can to obtain the nanometer powder of narrow diameter distribution;
(2) provided by the invention method is simple, simple to operate, and do not need the density adjusting solvent in mixed system, Success rate of virus isolation is high;
(3) equipment of the method use is conventional, with low cost;
(4) the solvent environmental protection that the method is used, environmental pollution is little;
(5) the method is easy to the post processing being separated the nano-powder obtained, and is easy to operation.
Embodiment
(1) mensuration of particle diameter of nanometer powder
The particle diameter of laser particle size method to nano-powder is used to measure in the present invention.
embodiment 1
(1) by the nano-tantalum of 0.2639g (assay balance weighing), (measuring its particle diameter by the method for () is 61.1 ~ 306.6nm, its grain-size graph is as shown in Figure 1) be scattered in 50mL ethylene glycol, fully disperse 30 minutes in ultrasonic machine, more scattered mixed liquor is loaded in centrifuge tube;
(2) at rotating speed be 1000rpm condition under centrifugal 30 minutes;
(3) upper liquid is shifted out separation system, by the centrifugal precipitum absolute ethanol washing obtained 3 times, vacuum drying 1 hour at 40 DEG C, again in absolute ethyl alcohol after ultrasonic disperse, the particle diameter of precipitum is measured by the method for (), its particle diameter is 240.7 ~ 303.6nm, and grain-size graph as shown in Figure 2;
(4) upper liquid continues at rotating speed is respectively 1500rpm, centrifugal 30min is carried out under the condition of 2000rpm and 2500rpm, repeat the operation of previous step 2 ~ 3, till upper liquid clarification, till the minimum grain size of powder that namely sedimentation obtains is the minimum grain size of nanometer powder to be separated.
Under rotating speed is 1500rpm, the particle diameter of the centrifugal nano-tantalum obtained is 164.9nm ~ 252.3nm, and grain-size graph as shown in Figure 3.
Under rotating speed is 2000rpm, the particle diameter of the centrifugal nano-tantalum obtained is 135.7nm ~ 171.2nm, and grain-size graph as shown in Figure 4.
Under rotating speed is 2500rpm, the particle diameter of the centrifugal nano-tantalum obtained is 71.4nm ~ 90.1nm, and grain-size graph as shown in Figure 5.
From embodiment 1, nano-tantalum can be scattered in ethylene glycol, successively to the centrifugal 30min of dispersion under the condition of 1000rpm, 1500rpm, 2000rpm and 2500rpm, 4 kinds of different-grain diameter grades can be obtained and the nano-tantalum of narrow diameter distribution, and, along with the increase of rotating speed, the particle diameter of the nano-tantalum obtained is less.
embodiment 2
(1) nano-tantalum (measuring its particle diameter by the method for () is 60.1 ~ 310.6nm) of 0.3998g (assay balance weighing) is scattered in 50mL Decanol, fully disperse 30 minutes in ultrasonic machine, more scattered mixed liquor is loaded in centrifuge tube;
(2) at rotating speed be 800rpm condition under centrifugal 40 minutes;
(3) upper liquid is shifted out separation system, by the centrifugal precipitum absolute ethanol washing obtained 3 times, vacuum drying 1 hour at 40 DEG C, then in absolute ethyl alcohol after ultrasonic disperse, measure the particle diameter of precipitum by the method for (), its particle diameter is 250 ~ 310nm;
(4) upper liquid continues at rotating speed is respectively 1300rpm, centrifugal 40min is carried out under the condition of 1800rpm and 2300rpm, repeat the operation of previous step 2 ~ 3, till upper liquid clarification, till the minimum grain size of powder that namely sedimentation obtains is the minimum grain size of nanometer powder to be separated.
Under rotating speed is 1300rpm, the particle diameter of the centrifugal nano-tantalum obtained is 180 ~ 240nm.
Under rotating speed is 1800rpm, the particle diameter of the centrifugal nano-tantalum obtained is 100 ~ 180nm.
Under rotating speed is 2300rpm, the particle diameter of the centrifugal nano-tantalum obtained is 60 ~ 80nm.
embodiment 3
(1) nano-tantalum (measuring its particle diameter by the method for () is 20.5 ~ 400.3nm) of 0.1325g (assay balance weighing) is scattered in 50mL ethanol-glycerol double solvents (viscosity is 100mPa.S), fully disperse 30 minutes in ultrasonic machine, more scattered mixed liquor is loaded in centrifuge tube;
(2) at rotating speed be 1200rpm condition under centrifugal 20 minutes;
(3) upper liquid is shifted out separation system, by the centrifugal precipitum absolute ethanol washing obtained 3 times, vacuum drying 1 hour at 40 DEG C, then in absolute ethyl alcohol after ultrasonic disperse, measure the particle diameter of precipitum by the method for (), its particle diameter is 150 ~ 200nm;
(4) upper liquid continues at rotating speed is respectively 1700rpm, centrifugal 20min is carried out under the condition of 2200rpm and 2700rpm, repeat the operation of previous step 2 ~ 3, till upper liquid clarification, till the minimum grain size of powder that namely sedimentation obtains is the minimum grain size of nanometer powder to be separated.
Under rotating speed is 1700rpm, the particle diameter of the centrifugal nano-tantalum obtained is 100 ~ 120nm.
Under rotating speed is 2200rpm, the particle diameter of the centrifugal nano-tantalum obtained is 50 ~ 80nm.
Under rotating speed is 2700rpm, the particle diameter of the centrifugal nano-tantalum obtained is 20 ~ 30nm.
comparative example 1
This comparative example method therefor is similar to embodiment 1, and difference is only that the particle diameter of nano-tantalum used is 1 ~ 20nm, and result cannot be separated nano-tantalum.
comparative example 2
This comparative example method therefor is similar to embodiment 2, and difference is only that the particle diameter of nano-tantalum used is 400 ~ 600nm, and result cannot be separated nano-tantalum.
comparative example 3
This comparative example method therefor is similar to embodiment 3, and difference is only that solvent for use is absolute ethyl alcohol (viscosity is 1.2mPa.S), and result nano-tantalum cannot disperse to form suspension in absolute ethyl alcohol, but all sedimentations.
comparative example 4
This comparative example method therefor is similar to embodiment 3, and difference is only that solvent for use is glycerine (viscosity is 1163mPa.S), and result nano-tantalum cannot be reunited in glycerine, rotating speed when increasing centrifugal, and tantalum powder also cannot sedimentation.
More than in conjunction with detailed description of the invention and exemplary example to invention has been detailed description, but these explanations can not be interpreted as limitation of the present invention.It will be appreciated by those skilled in the art that when not departing from spirit and scope of the invention, can carry out multiple equivalencing, modification or improvement to technical solution of the present invention and embodiment thereof, these all fall within the scope of the present invention.Protection scope of the present invention is as the criterion with claims.
Claims (10)
1. be separated a method for different-grain diameter nano particle, it is characterized in that, the method comprises the following steps:
(1) nanometer powder to be separated is scattered in solvent;
(2) dispersion step 1 obtained carries out centrifugation;
(3) shift out step 2 and obtain mixture liquid at the middle and upper levels, the precipitum obtained in step 2 is washed, dry;
(4) upper liquid shifted out in step 3 is repeated to the operation of step 2 ~ 3, until nanometer powder to be separated is completely separated.
2. method according to claim 1, is characterized in that, in step 1, the particle diameter of described nanometer powder to be separated is 20nm ~ 400nm, is preferably 60nm ~ 310nm.
3. method according to claim 1 and 2, is characterized in that, in step 1, described nanometer powder to be separated is nano zine oxide, nanometer aluminium powder, nano-tantalum.
4. according to the method one of claims 1 to 3 Suo Shu, it is characterized in that, in step 1, described nanometer powder to be separated is nano-tantalum, and being preferably particle diameter is 20nm ~ 400nm, is more preferably the nano-tantalum of 60nm ~ 310nm.
5. according to the method one of Claims 1 to 4 Suo Shu, it is characterized in that, in step 1, the viscosity of described solvent is 10mPa.s ~ 120mPa.s (16 DEG C), be preferably 20mPa.s ~ 70mPa.s (16 DEG C), be more preferably 20mPa.s ~ 40mPa.s (16 DEG C).
6., according to the method one of Claims 1 to 5 Suo Shu, it is characterized in that, in step 1, described solvent molecule is deposited hydroxyl, ehter bond, sulphur atom, oxygen atom or nitrogen-atoms etc. can with the functional group of metal-complexing.
7. according to the method one of claim 1 ~ 6 Suo Shu, it is characterized in that, in step 1, described solvent is ethylene glycol, Decanol or ethanol-glycerol double solvents, preferred ethylene glycol.
8. according to the method one of claim 1 ~ 7 Suo Shu, it is characterized in that, in step 1, the amount ratio of nanometer powder to be separated and solvent is the weight of nanometer powder to be separated: volume=(0.1 ~ 0.4) weight portion of solvent: 50 parts by volume, be preferably (0.2 ~ 0.3) weight portion: 50 parts by volume, wherein
Count 1 weight portion based on 1g, count 1 parts by volume based on 1mL.
9. according to the method one of claim 1 ~ 8 Suo Shu, it is characterized in that, in step 2, be 20nm ~ 400nm when nanometer powder to be separated is particle diameter, be preferably the nano-tantalum of 60nm ~ 310nm, when solvent for use is ethylene glycol, centrifugal rotating speed is 800 ~ 1200rpm, be preferably 1000rpm, centrifugation time is 20 ~ 40min, is preferably 30min.
10. according to the method one of claim 1 ~ 9 Suo Shu, it is characterized in that, in step 2, the rotating speed first during centrifugation is 800 ~ 1200rpm, and be preferably 1000rpm, centrifugation time is 20 ~ 40min, is preferably 30min; And/or
In step 4,
The rotating speed selecting centrifugation when second time is separated is 1300 ~ 1700rpm, and be preferably 1500rpm, centrifugation time is 20 ~ 40min, is preferably 30min; And/or
The rotating speed selecting centrifugation when third time is separated is 1800 ~ 2200rpm, and be preferably 2000rpm, centrifugation time is 20 ~ 40min, is preferably 30min; And/or
The rotating speed selecting centrifugation when being separated for the 4th time is 2300 ~ 2700rpm, and be preferably 2500rpm, centrifugation time is 20 ~ 40min, is preferably 30min.
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