CN106140450B - Microsphere separation device and separation method thereof - Google Patents
Microsphere separation device and separation method thereof Download PDFInfo
- Publication number
- CN106140450B CN106140450B CN201610595495.6A CN201610595495A CN106140450B CN 106140450 B CN106140450 B CN 106140450B CN 201610595495 A CN201610595495 A CN 201610595495A CN 106140450 B CN106140450 B CN 106140450B
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- Prior art keywords
- microballoon
- staving
- portals
- msub
- mrow
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- 239000004005 microsphere Substances 0.000 title claims abstract description 37
- 238000000926 separation method Methods 0.000 title claims abstract description 30
- 238000004062 sedimentation Methods 0.000 claims abstract description 30
- 238000005070 sampling Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims description 19
- 238000001514 detection method Methods 0.000 claims description 6
- 230000007246 mechanism Effects 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 5
- 239000005337 ground glass Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 abstract description 7
- 238000000746 purification Methods 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 description 8
- 238000011160 research Methods 0.000 description 4
- 230000006872 improvement Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 229920001002 functional polymer Polymers 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 102400000830 Saposin-B Human genes 0.000 description 1
- 101800001697 Saposin-B Proteins 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009795 derivation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009510 drug design Methods 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 238000003018 immunoassay Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B5/00—Washing granular, powdered or lumpy materials; Wet separating
- B03B5/28—Washing granular, powdered or lumpy materials; Wet separating by sink-float separation
- B03B5/30—Washing granular, powdered or lumpy materials; Wet separating by sink-float separation using heavy liquids or suspensions
- B03B5/36—Devices therefor, other than using centrifugal force
Landscapes
- Sampling And Sample Adjustment (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention provides a microsphere separation device and a separation method which have high separation precision and high yield and are suitable for large-scale application. The polymer microspheres with highly uniform particle sizes are obtained by separation and purification by using a sedimentation gradient method in combination with the device of the invention, and the method is applicable to separation of microspheres with any size; the separation precision and the yield are high; the microsphere outlet and the sampling microsphere outlet are arranged, so that the tracking of the separation process and the collection of the separation end are facilitated.
Description
Technical field
The present invention relates to a kind of separator more particularly to a kind of microballoon separator and its methods.
Background technology
Monodisperse polymer micro-sphere has been widely used bioanalysis, high-throughput detection, immunoassay and micro-total analysis system
The multiple fields such as system.Uniform particle sizes' degree of polymer microballoon has a significant impact to its performance, and most researchers pass through improvement side
Method controls technological parameter, can obtain particle diameter distribution than more uniform microballoon, it is common prepare mono-dispersion microballoon method have it is scattered
Polymerization, seeding polymerization and emulsion polymerization etc., but in fact, polymer microballoon in preparation process, since polymerisation always exists
It is carried out on boundary, though in system based on a kind of mechanism, exists simultaneously many secondary polymerization methods, and it is total in polymerization process
It is inevitable there are temperature change and monomer absorption process, these can all cause the microspherulite diameter finally synthesized distribution to become
It is wide.
Particularly, for seeding polymerization, the microballoon of synthesis always contains the smaller microballoon of some grain sizes (secondary core grade) and one
A little larger microballoons of grain size, this has seriously affected the dispersion degree of microballoon, limits the application of microballoon, it is therefore desirable to separating for several times with
Unwanted fraction in removing system.Common centrifugal separation method, based on different-grain diameter microballoon in centrifugal force field
Sedimentation time difference is separated, can only be excessive tentatively in removal system due to the centrifugal speed for being difficult to select to verify and time
Very small particle hardly results in the polymer microballoon of grain size high uniformity；Continuous-flow centrifugation can continuous separating-purifying
Polymer microballoon, but its separation accuracy is not high, to improve the uniformity coefficient of microballoon fraction, generally requires that separation is repeated several times,
The yield for causing microballoon is very low, and the microballoon needed additionally, due to this method is on a grand scale, it is difficult to realize small-scale application；Yoon
D H etc. realize the separating-purifying of microballoon using eddy channel partition method in the chips, but be limited to chip separation scale and into
This, is not suitable for scale application.And it is all in the prior art, the separation process of microballoon can not inspect sampling by random samples, be unfavorable for
The tracking of separation process.
In view of the above shortcomings, the designer, is actively subject to research and innovation, to found a kind of microballoon separator,
Make it with more the utility value in industry.
The content of the invention
In order to solve the above technical problems, the object of the present invention is to provide a kind of separation accuracy height, high income, suitable for scale
The microballoon separator of application.
The microballoon separator of the present invention, including staving, the staving has bucket bottom, staving side wall and bung hole, described
Staving side wall offers the microballoon microballoon that portals and inspect by random samples and portals respectively, and the sampling observation microballoon, which portals, is arranged on what the microballoon portalled
Upside and the two are both provided with valve, and the capacity of the staving is 1mL-10L, and the staving side wall is additionally provided with control mark
Line, the height h of the control tag line3It can be obtained by equation below：
Wherein, x is to load limit level, RDAnd RLThe respectively radius of the radius of targeted microspheres and larger microballoon, ρm、ρD
And ρLThe respectively apparent density of sedimentation liquid, targeted microspheres and larger microballoon, k are separation, numerical value between 0.5-1,
The selection of middle k values depends on separation requirement：If highly homogeneous microballoon is obtained, k values may be set to 0.5；It is separated if improving
Efficiency, k values may be set to 1.
Further, the microballoon microballoon that portals and inspect by random samples portals that be respectively equipped with relatively described staving side wall outwardly directed
First branch pipe and the second branch pipe, the valve are arranged in first branch pipe and the second branch pipe.
Further, matched dustproof cover is equipped at the bung hole.
Further, the dustproof cover is equipped with sealing mechanism with the bung hole contact position.
Further, the sealing mechanism is the ground glass on the inside of the dustproof cover and on the outside of the bung hole.
Further, the staving diameter d and staving height h ratios are d:H=1:0.5-50 is preferably d:H=2.
Further, the microballoon portals to the distance h at the bucket bottom1Portal with sampling observation microballoon to the distance at the bucket bottom
h2Ratio be h1:h2=1:1.5-2 it is preferably h1:h2=1:1.5, and h2Between the 1/10-1/3 of staving height h, preferably
1/4-1/3。
Further, the staving side wall is equipped with and loads upper limit tag line, loads lower limit tag line and control tag line,
Useful load is being loaded between upper limit tag line and loading lower limit tag line in the staving, preferably the nominal volume of 60-80%.
Further, the control tag line height h3Higher than h2, and several can be set, the control that staving mark can be replaced
Line paster processed, 1-20 control line of mark, each control line are located at different height respectively simultaneously on paster.
The method using microballoon separator separation microballoon of the present invention, comprises the following steps：
(1) microballoon and sedimentation liquid mixing are placed in the staving, stood；
(2) after the sedimentation boundary of targeted microspheres portals less than microballoon, the valve that microballoon portals is opened, is discharged compared with small particle
Microballoon, add in sedimentation liquid, repeat 3-20 time, when targeted microspheres sedimentation boundary reach control tag line when, from inspect by random samples microballoon
Portal sampling observation tracing detection, until accounting of the small particle microballoon in discharged microballoon is less than 1%；
(3) sedimentation liquid is added in, when the sedimentation boundary of targeted microspheres reaches control tag line, is portalled 4 pumpings from sampling observation microballoon
Tracing detection is examined, while portals from microballoon and discharges targeted microspheres, adds in sedimentation liquid, is repeated 3-10 times, sampling observation finally once divides
From microballoon in smaller and larger microballoon accounting be not higher than 1%.
Movement of the microballoon in liquid is had studied first, microballoon has been derived in liquid phase suspension, in constant gravitational field
Movement velocity formula, with reference to the doctoral thesis " research of monodisperse functional polymer microsphere " of University Of Tianjin Zhang Qi in 2010,
Wherein chapter 4 explicitly indicates that, finds the movement velocity of microballoon and the density of itself, diameter, suffered acceleration and solution
Property it is related；On the basis of accurately measurement glycerine water solution density and viscosity, a kind of milligram of magnitude is invented and has measured polymerization
The method of object Microsphere Density；Then SOLUTION PROPERTIES flow cytometric is had studied with the influence of microballoon signal in detecting.In microballoon liquid
On the basis of state suspended motion, sedimentation gradient method is developed.
According to the above aspect of the present invention, the present invention has at least the following advantages：
Sedimentation gradient method combination the device of the invention, isolates and purifies to obtain the polymer microballoon of grain size high uniformity.It utilizes
Available for isolating and purifying for milligram grade quantum dot coding fluorescence microballoon, it is micro- to improve fluorescence for apparatus of the present invention combination sedimentation gradient method
The analysis precision of ball.
The microballoon separator of the present invention is applicable to the microballoon separation of any scale；And separation accuracy is high, yield
It is high；Portal equipped with microballoon and inspect microballoon by random samples and portal and control line, convenient for the collection that terminates of tracking and separation of separation process.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, below with presently preferred embodiments of the present invention and coordinate attached drawing be described in detail as after.
Description of the drawings
Fig. 1 is a kind of structure diagram of embodiment of apparatus of the present invention.
Specific embodiment
With reference to the accompanying drawings and examples, the specific embodiment of the present invention is described in further detail.Implement below
Example is not limited to the scope of the present invention for illustrating the present invention.Referring to Fig. 1, a kind of microballoon separator of the invention, bag
Include staving, the staving has bucket bottom 2, staving side wall 1 and a bung hole 13, and the staving side wall 1 offers microballoon and portals 3 respectively
Portal 4 with sampling observation microballoon, the sampling observation microballoon, which portals, 4 is arranged on that the microballoon portals 3 upside and the two is both provided with valve
Door 7, the capacity of the staving is 1mL-10L, and the staving side wall 1 is additionally provided with control tag line 12, the control tag line 12
Height h3It can be obtained by equation below：
Wherein, x is to load limit level, RDAnd RLThe respectively radius of the radius of targeted microspheres and larger microballoon, ρm、ρD
And ρLThe respectively apparent density of sedimentation liquid, targeted microspheres and larger microballoon, the selection of k values depend on separation requirement：If k values are set
It is set to 0.5, separated efficiency is about the 40-50% of highest separative efficiency, the C of thus obtained microsphereV(relative standard deviation) is less than
3%；Lower (being less than 0.5) if of the setting of k values, the C of thus obtained microsphereVIt can further improve, but separated efficiency can be reduced greatly；
If k values are set as 1, separated efficiency is about the 80-95% of highest separative efficiency, the C of thus obtained microsphereVLess than 8%；If k values are set
It is set between 0.5-1, then the C of separated efficiency and microballoonVBetween above-mentioned numerical value；Particularly, k values are set as 0.7, separation
Number 8 times, gained separative efficiency are about the 65% of highest separative efficiency, the C of thus obtained microsphereVLess than 4%, the yield of microballoon is
22-32%；Highest separative efficiency is the attainable separation peak of this separator, and in this state, the yield of microballoon is
35-50%.
For convenience of sampling observation microsphere sample and separating obtained microballoon is collected, and does not upset layering, the microballoon portals 3 and pumping
Inspection microballoon, which portals, 4 is respectively equipped with relatively described 2 outwardly directed first branch pipe, 5 and second branch pipe 6 of staving side wall, the valve 7
In 5 and second branch pipe 6 of the first branch pipe.
Foreign matter enters in staving in order to prevent, and prevents staving internal solvent from volatilizing, and is equipped at the bung hole 13 matched
Dustproof cover 8.
In order to preferably prevent staving internal solvent from volatilizing, the dustproof cover 8 is equipped with sealer with 13 contact position of bung hole
Structure.
Preferably, the sealing mechanism is the ground glass 9 arranged on 13 outside of 8 inside of dustproof cover and the bung hole.
According to hydrodynamics, liquid can be disturbed by crossing major diameter, influence separating effect, reduce yield, the staving diameter d with
Staving height h ratios are d:H=1:0.5-50 is preferably d:H=2.
The microballoon portal 3 arrive the bucket bottom 2 distance h1With sampling observation microballoon portal 4 arrive the bucket bottom 2 distance h2Ratio
Example is h1:h2=1:1.5-2 it is preferably h1:h2=1:1.5, and h2Between the 1/10-1/3 of staving height h, optimum height is about
For 1/4-1/3, rational design can optimize separative efficiency.
Preferably, the staving side wall is equipped with and loads upper limit tag line 10, loads lower limit tag line 11 and control mark
Line 12, useful load is between loading upper limit tag line 10 and loading lower limit tag line 11 in the staving, the preferred volume of 60-80%
Constant volume.
12 position of control tag line is mainly determined by sedimentation liquid density and targeted microspheres size, too high or too low, can be dropped
Low yield, the 12 height h of control line3Higher than h2, with reference to the doctoral thesis of University Of Tianjin Zhang Qi in 2010, " monodisperse function is gathered
The derivation of equation in chapter 4 in the research of conjunction object microballoon " draws control tag line specific location.
When apparatus of the present invention is used to separate microballoon, staving marks the interchangeable translucent paster of control line, according to grain size
It is of different sizes, the control line of different target microballoon is set, if targeted microspheres to be separated are 2.5 μm of dispersin polymerization thus obtained microsphere,
Control line is arranged at the 2/5 of staving (k values are about 0.9), separative efficiency 45%；If targeted microspheres to be separated are 10 μm of kind
Son polymerization thus obtained microsphere, control line are arranged at the 1/4 of staving (k values are about 0.7), separative efficiency 22%；First, by microballoon
It is placed on sedimentation liquid mixing in the staving of apparatus of the present invention, covers dustproof cover 8, stood, when the sedimentation boundary of targeted microspheres is low
Portal in microballoon after 3, open valve 7, discharge the microballoon compared with small particle, add in sedimentation liquid, repeat the process 3-20 times, work as target
When the sedimentation boundary of microballoon reaches control tag line 12, portal 4 sampling observation tracing detections from sampling observation microballoon, until small particle microballoon exists
Accounting in institute's discharge microballoon is less than 1%；Then, sedimentation liquid is added in, when the sedimentation boundary of targeted microspheres reaches control tag line
When 12, portal 4 sampling observation tracing detections from sampling observation microballoon, while portal 3 discharge targeted microspheres from microballoon, add in sedimentation liquid, repeat
Process 3-10 times；In the final once separated microballoon of sampling observation, smaller and larger microballoon accounting is not higher than 1%；Specific method
With reference to University Of Tianjin Zhang Qi in 2010 doctoral thesis " research of monodisperse functional polymer microsphere " in chapter 4.
The above is only the preferred embodiment of the present invention, is not intended to limit the invention, it is noted that for this skill
For the those of ordinary skill in art field, without departing from the technical principles of the invention, can also make it is several improvement and
Modification, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of microballoon separator, including staving, the staving has bucket bottom, staving side wall and bung hole, it is characterised in that：
The staving side wall offers the microballoon microballoon that portals and inspect by random samples and portals respectively, and the sampling observation microballoon, which portals, to be arranged on the microballoon and go out
The upside in hole and the two are both provided with valve, and the staving side wall is additionally provided with control tag line, the height of the control tag line
Spend h3It can be obtained by equation below：
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<mi>k</mi>
<mo>&CenterDot;</mo>
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<mo>&CenterDot;</mo>
<mfrac>
<mrow>
<msubsup>
<mi>R</mi>
<mi>D</mi>
<mn>2</mn>
</msubsup>
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<mo>(</mo>
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<mi>&rho;</mi>
<mi>m</mi>
</msub>
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<mi>&rho;</mi>
<mi>D</mi>
</msub>
<mo>)</mo>
</mrow>
</mrow>
<mrow>
<msubsup>
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Wherein, x is to load limit level, RDAnd RLThe respectively radius of the radius of targeted microspheres and larger microballoon, ρm、ρDAnd ρLPoint
Not Wei sedimentation liquid, targeted microspheres and larger microballoon apparent density, k is separation, and numerical value is between 0.5-1.
2. microballoon separator according to claim 1, it is characterised in that：The microballoon microballoon that portals and inspect by random samples portals point
It She You not outwardly directed first branch pipe of relatively described staving side wall and the second branch pipe.
3. microballoon separator according to claim 1, it is characterised in that：It is equipped at the bung hole matched dust-proof
Lid.
4. microballoon separator according to claim 3, it is characterised in that：The dustproof cover is set with the bung hole contact position
There is sealing mechanism.
5. microballoon separator according to claim 4, it is characterised in that：The sealing mechanism is arranged on the dustproof cover
Ground glass on the outside of inside and the bung hole.
6. microballoon separator according to claim 1, it is characterised in that：The staving diameter d and staving height h ratios
For d:H=1:0.5-50.
7. microballoon separator according to claim 1, it is characterised in that：The microballoon portals to the distance at the bucket bottom
h1Portal with sampling observation microballoon to the distance h at the bucket bottom2Ratio be h1:h2=1:1.5-2 and h2In the 1/10- of staving height h
Between 1/3.
8. microballoon separator according to claim 1, it is characterised in that：The staving side wall, which is equipped with, loads upper limit mark
Line loads lower limit tag line and control tag line.
9. microballoon separator according to claim 1, it is characterised in that：The control tag line height h3Higher than h2, and
Several can be set.
10. utilize the method for the microballoon separator separation microballoon as described in claim 1 to 9 is any, which is characterized in that including
Following steps：
(1) microballoon and sedimentation liquid mixing are placed in the staving, stood；
(2) after the sedimentation boundary of targeted microspheres portals less than microballoon, the valve that microballoon portals is opened, is discharged micro- compared with small particle
Ball adds in sedimentation liquid, repeats 3-20 times, when the sedimentation boundary of targeted microspheres reaches control tag line, portals from sampling observation microballoon
Tracing detection is inspected by random samples, until accounting of the small particle microballoon in discharged microballoon is less than 1%；
(3) add in sedimentation liquid, when targeted microspheres sedimentation boundary reach control tag line when, from sampling observation microballoon portal 4 sampling observations with
Track detects, while portals from microballoon and discharge targeted microspheres, adds in sedimentation liquid, repeats 3-10 times, and sampling observation is final once separated
Smaller and larger microballoon accounting is not higher than 1% in microballoon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610595495.6A CN106140450B (en) | 2016-07-27 | 2016-07-27 | Microsphere separation device and separation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610595495.6A CN106140450B (en) | 2016-07-27 | 2016-07-27 | Microsphere separation device and separation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106140450A CN106140450A (en) | 2016-11-23 |
| CN106140450B true CN106140450B (en) | 2018-05-25 |
Family
ID=58059882
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|---|---|---|---|
| CN201610595495.6A Active CN106140450B (en) | 2016-07-27 | 2016-07-27 | Microsphere separation device and separation method thereof |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110548328A (en) * | 2019-08-26 | 2019-12-10 | 浙江圣兆药物科技股份有限公司 | Microsphere screen mesh, production type efficient microsphere collecting device and application thereof |
| CN111437984A (en) * | 2019-12-31 | 2020-07-24 | 武汉理工大学 | Elutriation method elutriation device and application thereof in single mineral classification of micro-fine particle oxidized ore |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2043163C1 (en) * | 1992-05-05 | 1995-09-10 | Фирма "Микросфера" | Hydraulic classifier |
| CN101712013A (en) * | 2008-10-06 | 2010-05-26 | 中国科学院大连化学物理研究所 | Method for classifying calcium alginate plastic beads |
| CN101716550A (en) * | 2009-11-16 | 2010-06-02 | 清华大学 | Microsphere separation method and screening system |
| CN202778681U (en) * | 2012-04-27 | 2013-03-13 | 河南新大新材料股份有限公司 | Micro powder automatic siphon size grading device |
| CN103008093A (en) * | 2012-12-05 | 2013-04-03 | 平顶山易成新材料股份有限公司 | Method for separating free carbon from ultra-fine silicon carbide powder |
| CN206139323U (en) * | 2016-07-27 | 2017-05-03 | 苏州大学 | Microsphere separation device |
-
2016
- 2016-07-27 CN CN201610595495.6A patent/CN106140450B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2043163C1 (en) * | 1992-05-05 | 1995-09-10 | Фирма "Микросфера" | Hydraulic classifier |
| CN101712013A (en) * | 2008-10-06 | 2010-05-26 | 中国科学院大连化学物理研究所 | Method for classifying calcium alginate plastic beads |
| CN101716550A (en) * | 2009-11-16 | 2010-06-02 | 清华大学 | Microsphere separation method and screening system |
| CN202778681U (en) * | 2012-04-27 | 2013-03-13 | 河南新大新材料股份有限公司 | Micro powder automatic siphon size grading device |
| CN103008093A (en) * | 2012-12-05 | 2013-04-03 | 平顶山易成新材料股份有限公司 | Method for separating free carbon from ultra-fine silicon carbide powder |
| CN206139323U (en) * | 2016-07-27 | 2017-05-03 | 苏州大学 | Microsphere separation device |
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