CN108051437A - A kind of high throughput polymeric detection method - Google Patents
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- CN108051437A CN108051437A CN201711144293.0A CN201711144293A CN108051437A CN 108051437 A CN108051437 A CN 108051437A CN 201711144293 A CN201711144293 A CN 201711144293A CN 108051437 A CN108051437 A CN 108051437A
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Abstract
The invention belongs to component of polymer detection technique fields, are related to the molten region altogether quickly detected in Polymer Blending System, and be separated region, are specially a kind of high-throughput polymeric detection method.The present invention passes through titration outfit and high-precision laser detection device, under series of temperature gradient, obtain respective nodes, according to gained each group of data, make binodal line and spinodal that binary high polymer system changes with solution concentration, solvable situation in the common solution system of two kinds of incompatible polymers of quantitative analysis and solvent, screens soluble ingredient.The present invention has the advantages of low cost, simple to operate.
Description
Technical field
The invention belongs to component of polymer detection technique field, be related to quickly detect it is molten altogether in Polymer Blending System
Region, be separated region, is specially a kind of high-throughput polymeric detection method.
Background technology
Phase separation method is to form one of new Process ba- sis of preparation microcapsules technology, and people will be given as a kind of new technology
Many novel products are provided, meet the various demands of people, there is broad prospect of application.With the rapid development of microcapsules technology,
Its application range also expands to medicine, food, pesticide, feed, ink, bonding from initial drug cladding and carbonless paper
The industries such as agent, cosmetics, detergent, photosensitive material, weaving obtain wide application.Exist especially with microcapsules technology
Biology, the popularization and application of medical domain, phase detachment technique are widely used in large-scale culture, cell and the enzyme of zooblast
Immobilization, the control release of drug, in terms of the separation of substances such as the screening of anticancer drug and protein.Pass through from nineteen sixty
Since phase inversion is prepared for first business cellulose acetate reverse osmosis film, be separated due to its efficient separating property and
Gradually substitute traditional chemical industry, bioseparation technology, be widely used at the industrial wastewater of food, beverage, plating, medicine field
In reason.
Phase separation method is exactly to generate different aggregation phases, shape by various means reaction solutions or aqueous solutions of polymers
It is separated into polymer rich phase and polymer-poor phase, removes solvent phase and leave hole in polymer matrix body.Fortune
With phase separation method, on the basis of coprecipitation, suitable surfactant is added, makes sediment using specific organic solvent
It is mutually separated with water into organic phase, achievees the purpose that separation of solid and liquid.Organic solvent through evaporating volatile is it is possible that obtain grain
Spend thin and scattered powdered solid electrolyte.Someone is prepared for superfines α-Al2O3 in this way at present.
It can be seen that phase detachment technique development prospect is wide, the demand of the new detecting method on phase separation is increasing.
It is existing phase separation detection method rely primarily on energy spectrum analysis, X-ray diffraction facies analysis, chromatography, mass spectral analysis, chromatography-
Mass spectrometry analysis, nuclear magnetic resonance technique, spectrum analysis.
Energy spectrum analysis is substantially power dissipation spectrum analysis, and the most commonly used is the analyses of Si (Li) X-ray energy spectrum, and critical component is
Si (Li) detector, analyze speed is fast, high sensitivity, but energy resolution is low, the peak back of the body is than low, and Si (Li) probes must be protected always
Hold liquid helium cooling low-temperature condition, even can not be interrupted when not working, otherwise in crystal Li concentration distribution state
It will change due to diffusion, probe function be caused to decline even completely destroyed, operating condition requirement is very harsh.
X-ray diffraction facies analysis (phase analysis of x ray diffraction) is in crystal using X-ray
Diffraction effect in substance carries out the technology of structure of matter analysis.But, when object mutually more spectral line higher to determinand purity requirement
, easily there is overlap of spectral lines in complexity, quantitative analysis difficult, and mathematical computations are cumbersome.
Chromatography is a kind of separation and analysis method, is distributed using selectivity of the different material in different phase, with stream
The dynamic mixture being relatively fixed in phase is eluted, and different substances can be moved along stationary phase at different rates in mixture,
It is finally reached separated effect.It is easy to operate quick, but separating effect is bad when separated object polarity spectrum is smaller, is separated
The selection of solvent and stationary phase is relatively difficult when object polarity size is uncertain, and when elution is more using solvent, and solvent can be caused unrestrained
Take.
Mass spectral analysis is to be separated substance ion by the mass-to-charge ratio of ion with electric field and magnetic field, then measure it is various from
The intensity of sub- spectral peak and realize a kind of analysis method of analysis purpose.Analytical reagent composition precision is higher, but the work period is long, needs
Sampling analysis belongs to destructive method of analysis.
Chromatograph-mass spectrometer coupling analysis is a kind of technology for being combined chromatography with mass spectral analysis, with high efficiency chromatography point
Analyse the sample introduction and piece-rate system as mass spectral analysis, detecting system of the mass spectral analysis as chromatography.Sample is in mass spectrum part
It is separated with flowing, after being ionized, separates fragment ion by charge-mass ratio through mass spectrographic mass analyzer, device obtains after testing
Mass spectrogram.Chromatograph-mass spectrometer coupling analysis can analyze many kinds of substance, but its work period is long, and systematic comparison is complicated, expensive,
Still it is a kind of destructive analysis.
Nuclear magnetic resonance technique can go deep under the premise of sample is not destroyed inside detecting material, be the chemical group for analyzing substance
Into, structure and its a kind of means of variation.Pretreatment is not required to complex sample to be analyzed, quickly, accurately.But expense is held high
Expensive, sweep time is long, and spatial resolution is not ideal enough, and sensitivity is relatively low.
Spectrum analysis is the spectrum generated with the interaction between electromagnetic radiation and the atom or molecule of substance, to differentiate
Substance and determine it chemical composition and relative amount a kind of method.Spectrum analysis is sensitive rapid, but for nonmetallic and boundary
In metal and it is nonmetallic between element be difficult accurately to detect, be not original method, it is impossible to as arbitration analysis method, detection knot
Fruit cannot be bought as national authentication foundation and maintenance cost is all higher, cost performance is relatively low, for small lot sample detection not
It corresponds to reality, is easily influenced by the outside or inside factor such as optical system parameter, curve nonlinear problem often occur, to testing result
Accuracy be affected.
The prior art has been respectively present the shortcomings of cost is higher, and operating condition is harsh, complicated in a word.
The content of the invention
For above-mentioned there are problem or deficiency, for solve can melt into the co-mixing system of two kinds of incompatible polymers and solvent
The problem of high cost existing for sorting survey, operating condition is harsh, complicated, the present invention provides a kind of high-throughput polymeric detection sides
Method.
The present invention under series of temperature gradient, is accordingly saved by titration outfit and high-precision laser detection device
Point according to gained each group of data, makes binodal line and spinodal that binary high polymer system changes with solution concentration, quantitative analysis
Solvable situation in the common solution system of two kinds of incompatible polymers and solvent, screens soluble ingredient.
It is as follows：
Step 1 is stirred the reactor for filling solution A and is heated to preset temperature, and keeps the temperature, while records reactor
The concentration of middle solution A, solution A are polymer solution.
Step 2 opens laser detector, and the titration of B solution is carried out to the solution A in reactor, is stirred in titration.
The laser of the transmitting terminal transmitting of the laser detector is received through solution in reactor by the receiving terminal of laser detector,
To detect the intensity signal by solution in reactor, B solution is polymer solution, and A, B solution are different and dissolve in identical
Solvent.
Step 3 persistently titrates B solution, and in this process, solution is become cloudy by limpid up to completely muddy in reactor,
Become limpid by completely muddy again；The laser intensity for recording the reception of first time laser pick-off end reaches when reaching setting value 1 and 2
The laser intensity that the amount of B solution and second of laser pick-off end receive reaches the amount of B solution when reaching setting value 1 and 2；
The laser intensity setting value 1 is light intensity of the laser through turbid solution in the limpid conversion with chaos state；Swash
Light light intensity setting value 2 is less than setting value 1, and more than the correspondence light intensity of complete turbid solution.
Step 4, the temperature for changing solution in reactor repeat step 1-3,2 arrival setting values 1 described in recording step 3
During with 2, the amount of B solution at 4 nodes.
Step 5, foundation step 3 and 4 the data obtaineds, draw binodal line of the binary high polymer system with the variation of solution concentration
With spinodal figure, the image hotpoint polymeric detection according to drafting.
Further, the reactor is at least one, and the solution A concentration in each reactor is different, to realize high pass
Amount.
The present invention makes full use of binary superpolymer blend phase separation mechanism：Fundamentally, the phase of superpolymer blend
Capacitive is by its (classics) thermodynamics essence, i.e. the variation △ G (mono- T △ S of=△ H) of gibbs (Gibbe) free energy are determined
's.According to thermodynamic principles, △ G<0 is compatible necessary condition.For high polymer system, if without intermolecular special phase
Interaction or Intramolecular repulsion, △ H are typically larger than zero, and △ S contributions are very small, so most high polymer blendings
System is all incompatible.Each tie point then gives the restrictive condition of compatible system, i.e. x2<B ' or x2>b”.Stationary point s ' and
S " defines unstable split-phase (sPiondal) condition, i.e. s '<x2<System is phase separation during s ".And concentration range is in b and s
Between when, system is metastable (iBondal).
Therefore, when the polymer A for being dissolved in solvent a kind of at the beginning adds in minute quantity polymer B, the two be it is compatible, with
Increasing for B content, the two enters meta-stable area, is then separated, and continues to increase B, to a certain concentration, the two phase again
Hold, by the Laser Detecting Set of quantitative titration device and direct light-intensity test mode, (direct detecting method is connect with receiver
The variation of the luminous flux received detects.When a branch of laser for being irradiated to reactor is had an X-rayed, it is possible to understand that be reaction solution microwave
Intensity modulated is carried out to laser beam, the laser transmitted away just carries reaction solution signal message, can be with according to signal message
Judge solution situation of change, changed correspondingly again to limpid corresponding light intensity to muddiness by limpid), it (is adopted using high-throughput Experimental Establishment
With multiple reactors), experiment condition system high throughput for the moment is realized, titration is simple and effective with detection device, reduces cost,
Operation is simplified, substantially increases the efficiency and experimental precision of experimental study.
The present invention, based on laser detector, realizes various concentration gradient and lower pair of temperature gradient using phase separation principle
The drafting of nodel line, spinodal figure reaches the technique effect of component of polymer detection.
In conclusion the present invention has the advantages of low cost, simple to operate.
Description of the drawings
Fig. 1 is the test iron plate top view of embodiment；
Fig. 2 is the side view of embodiment；
Fig. 3 is to change with solution A concentration, the binary high polymer system free energy of mixing and binodal line, spinodal correspondence
Figure；
Reference numeral:1-test iron plate, 2-hole, 3-titration outfit, 4-buret, 5-stent, 6-laser hair
Injection device, 7-temperature controller, 8-oil, 9-parallel blender, 10-stirrer, 11-test tube, 12-laser pick-off dress
It puts, 13-solution A, 14-B solution.
Specific embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.
The test iron plate (1) of 8 (a) × 8 (a) is placed as shown in Figure 1, and test iron plate opens 64 holes (2)；Such as Fig. 2 institutes
Show holding test tubes (11) i.e. reactor, to test tube oil bath heating.Simultaneously iron plate (1) is tested to be placed on parallel blender (9),
Under the collective effect of the internal stirrer (10) of test tube (11), realization is rapidly and uniformly stirred.
It tests iron plate (1) upper left corner and places temperature controller (7), realize the control and adjustment of test temperature.Test tube (11)
Mixed solution (13) the i.e. solution A of A polymer and solvent C is inside placed with, A polymer is dissolved in C solvents.It is mixed in test tube (11)
Liquid (13) liquid level is closed higher than test iron plate (1) upper surface.Each test tube both sides placed laser beam emitting device (6) and laser respectively
Reception device (12), stream oriented device are connected by stent (5) with titration outfit (3).
The lower section of test tube (11) face buret (4), the buret (4) on titration outfit (3) are being located at test tube (11) just
Top, buret lower section nozzle prevent liquid from spilling, buret (4) receives poly- from titration outfit (3) less than edge on test tube
Close mixed solution (14) the i.e. B solution of object B and solvent C.Polymer B is incompatible with polymer A, but dissolves in solvent C.Titration dress
It is controllable to put switch, while quantitative measurment can be realized to titrating solution, rate of titration control is 9ml/min.
After all devices are placed correctly, solution A (13) is added in test tube (11), liquid level is higher than test iron plate (1)
Upper surface.At this point, A dissolves in solvent C, and with definite concentration gradient, the content for recording A in corresponding solution at this time is respectively
a1、a2、a3……a64。
It is operated using foregoing detection method.It is T by the temperature setting of temperature controller (7), titration starts, B solution
(14) when infusion volume is few, solution A (13) is still limpid in test tube (11), through reactor laser by laser receiver
(12) receive and obtain intensity signal；In titration process, with the increase of B solution (14) titer, polymer A is incompatible with B,
It is separated, muddiness occurs in solution, and the light intensity of reception device (12) reaches preset value 1, records B in corresponding solution at this time
Content for b1 (1), b2 (1), b3 (1) ... b64 (1)；The laser intensity received to receiving terminal reaches setting value 2, right at this time
The content of B is b1 (2), b2 (2), b3 (2) ... b64 (2) in the solution answered；With the lasting progress of titration, sometime
Solution becomes limpid from muddiness, and the laser intensity that receiving terminal receives reaches setting value 2, writes down the content b1 of B in solution at this time
(3)、b2(3)、b3(3)……b64(3)；The laser intensity to be received that receive that terminates reaches setting value 1, writes down B in solution at this time
Content b1 (4), b2 (4), b3 (4) ... b64 (4).One group of experiment terminates at this time.
In the case where other conditions are constant, temperature is adjusted, is repeated the above steps, formed temperature gradient, draw corresponding data, make
The binodal line and spinodal changed such as Fig. 3 binary high polymer system with solution A concentration, you can two kinds of incompatible polymerizations of quantitative analysis
Solvable situation, is detected soluble ingredient in the co-mixing system of object and solvent, △ GmFor the change of gibbs (Gibbe) free energy
Change amount, △ μ1、△μ2For voltage variety.
To sum up, the present invention is easy to operate, of low cost, can quickly realize different temperatures gradient, various concentration ladder
The detection of the soluble ingredient of degree.
Claims (2)
1. a kind of high throughput polymeric detection method, is as follows：
Step 1 is stirred the reactor for filling solution A and is heated to preset temperature, and keeps the temperature, while records A in reactor
The concentration of solution, solution A are polymer solution；
Step 2 opens laser detector, and the titration of B solution is carried out to the solution A in reactor, is stirred in titration；It is described
The laser of the transmitting terminal transmitting of laser detector is received through solution in reactor by the receiving terminal of laser detector, with inspection
The intensity signal by solution in reactor is surveyed, B solution is polymer solution, and A, B solution are different and dissolve in identical solvent；
Step 3 persistently titrates B solution, and in this process, solution is become cloudy by limpid up to complete muddiness in reactor, then by
It is completely muddy to become limpid；It is molten to record the B that the laser intensity that first time laser pick-off end receives reaches when reaching setting value 1 and 2
The laser intensity that the amount of liquid and second of laser pick-off end receive reaches the amount of B solution when reaching setting value 1 and 2；
The laser intensity setting value 1 is light intensity of the laser through turbid solution in the limpid conversion with chaos state；Laser light
Strong setting value 2 is less than setting value 1, and more than the correspondence light intensity of complete turbid solution；
Step 4, the temperature for changing solution in reactor repeat step 1-3,2 arrival setting values 1 and 2 described in recording step 3
When, the amount of B solution at 4 nodes；
Step 5, foundation step 3 and 4 the data obtaineds draw binodal line and rotation of the binary high polymer system with the variation of solution concentration
Nodel line figure, according to the image hotpoint polymeric detection drawn.
2. high throughput polymeric detection method as described in claim 1, it is characterised in that：The reactor is at least one, and each
Solution A concentration in reactor is different.
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| US20100216946A1 (en) * | 2007-09-27 | 2010-08-26 | Hiroshi Takahashi | Polymer alloy and production method thereof |
| CN101952051A (en) * | 2008-02-19 | 2011-01-19 | 富士胶片株式会社 | Multilayer film and manufacturing method thereof |
| US20130334123A1 (en) * | 2008-11-21 | 2013-12-19 | 3M Innovative Properties Company | Microporous membrane and method for forming |
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2017
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| US20090286894A1 (en) * | 2006-04-07 | 2009-11-19 | Justin John Cooper-White | Porous polymer blend structures |
| US20100216946A1 (en) * | 2007-09-27 | 2010-08-26 | Hiroshi Takahashi | Polymer alloy and production method thereof |
| CN101952051A (en) * | 2008-02-19 | 2011-01-19 | 富士胶片株式会社 | Multilayer film and manufacturing method thereof |
| CN101952051B (en) * | 2008-02-19 | 2013-08-07 | 富士胶片株式会社 | Multilayer film and manufacturing method thereof |
| US20130334123A1 (en) * | 2008-11-21 | 2013-12-19 | 3M Innovative Properties Company | Microporous membrane and method for forming |
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