CN101531767B - Micro-nano granules dispersion method in polymer basal body using liquid-liquid interface - Google Patents
Micro-nano granules dispersion method in polymer basal body using liquid-liquid interface Download PDFInfo
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- CN101531767B CN101531767B CN200910113999XA CN200910113999A CN101531767B CN 101531767 B CN101531767 B CN 101531767B CN 200910113999X A CN200910113999X A CN 200910113999XA CN 200910113999 A CN200910113999 A CN 200910113999A CN 101531767 B CN101531767 B CN 101531767B
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Abstract
The invention discloses a micro-nano granules dispersion method in polymer basal body using liquid-liquid interface. SiO2 micro or nano granules are synthesized using chemical method and prepared into alcohol colloidal solution using centrifugal separation and ultrasonic dispersion; the alcohol colloidal solution is added into toluene/water liquid-liquid interface and the micro-nano granules uniformly disperse using the physicochemical characteristics of the interface; the polymer monomer dissolves in the organic solvent immiscible with water and initiator dissolves in the buffer solution. The local polymerization reaction on the liquid-liquid interface is initiated to generate polymer/SiO2 granule polymer film; the prepared polymer/SiO2 granule polymer film and the polymer blank film without SiO2 are subjected to pressure forming, therefore the polymer composite material with uniformly dispersed SiO2 micro-nano granules is produced. The technique method is simple and the problem is solved that the micro-nano granules difficultly disperse in the polymer basal body and easily coagulate.
Description
Technical field
The present invention relates to a kind of liquid-liquid interface that utilizes and carry out micro-nano granules dispersive method in polymeric matrix.
Background technology
Polymer matrix composite has been widely used in fields such as industry, national defence and aerospace at present.Bibliographical information adds nano particle (as SiO in polymeric matrix
2Nano particle) can significantly improve the mechanical property of polymeric matrix.Polymeric matrix after the modification can also be further carries out compoundly with other various fillers or toughener, makes the high performance polymer composite material with practical value.But nano particle is difficult to disperse in polymeric matrix owing to have bigger serface and surfactivity, is easy to occur clustering phenomena, thereby influences modified effect.Utilize micro-nano granules characterization of adsorption and dissemination on the profit liquid-liquid interface,, can effectively prevent to reunite, realize the homodisperse of micro-nano granules in polymeric matrix, make polymkeric substance/micro-nano granules composite membrane by the polymerized in-situ method.The multi-disc composite membrane can and then prepare polymkeric substance/micro-nano granules matrix material through compression molding.The method of disperseing micro-nano granules to prepare polymkeric substance/micro-nano granules matrix material with liquid-liquid interface yet there are no report at present.
Summary of the invention
Purpose of the present invention just provides a kind of micro-nano granules dispersive method in polymeric matrix.The steps include:
1, with the tetraethoxy being main raw material, is ammoniacal liquor, 50-55ml dehydrated alcohol and the mixing of 100ml redistilled water of 25%-28% with the 160-175ml volume percent, stirs 3-10 minute in the constant temperature magnetic stirrer, dropwise adds 18-22ml again with SiO
2The meter volume percent is the tetraethoxy of 20%-30%, continues to stir 5-48 hour, and control reaction temperature is between 12-30 ℃; Product changes with 3000 and carries out centrifugation, after the gained precipitation washing three times in ethanol ultra-sonic dispersion 20-60min, obtain SiO
2Colloidal sol;
2, the 3-6ml organic monomer is dissolved in 30-60ml and the immiscible organic solvent of water, make organic solution, described organic solvent is a kind of in toluene, benzene and the oil of mirbane, and described organic monomer is a kind of in vinylbenzene and the aniline; Get redistilled water 30-60ml, add 1.5-2.5g organic monomer polymerization starter and make initiator solution A, described organic monomer polymerization starter is a Potassium Persulfate; In the 30-60ml redistilled water, dissolve 0.06-0.10g NaHCO in addition
3Make buffered soln B;
3, organic solution that equal-volume step (2) is made and buffering solution B are put into beaker and are left standstill 5-10min to two and be separated, and drip the SiO that 2-20ul step (1) makes at liquid-liquid interface
2Colloidal sol; Treat SiO behind the 4-20min
2Particle is after liquid-liquid interface disperses to finish, and the initiator solution A that 1-3mL step (2) is made directly injects water with pipettor, causes the polymerized in-situ reaction; After 24 hours, the composite membrane that floats over liquid-liquid interface is shifted out, make and contain SiO
2The particulate polymeric film; Do not add SiO in addition
2Colloidal sol prepares blank polymeric film with identical step;
What 4, step (3) is made contains SiO
2SiO is prepared in particulate polymeric film and blank polymeric film compression molding
2The homodisperse polymer composites of nano particle.
Concrete feature of the present invention:
(1) SiO
2Nano particle can make nano particle fully be disperseed after introducing the profit liquid-liquid interface by colloidal sol.
(2) SiO
2The content of nano particle in polymkeric substance can pass through SiO
2The addition of colloidal sol is adjusted.
(3) on-site polymerization helps to realize well compound between nano particle and the polymeric matrix.
Technology of the present invention is simple, and nano particle fully disperses in polymeric matrix, and the addition controllability is strong, and may realize the continuous output of polymeric film by the device design, has solved nano particle effectively and has disperseed difficult problem at polymeric matrix.
Embodiment
Embodiment:
1, with the tetraethoxy is main raw material, ammoniacal liquor, the 51.2ml volume percent that with the 168ml volume percent is 25%-28% earlier is 99.7% ethanol and the mixing of 100ml redistilled water, in the constant temperature magnetic stirrer, stirred 5 minutes, and dropwise added the 20ml volume percent again and be 28.0% (with SiO
2Meter) tetraethoxy with 60 rev/mins rotating speed, continues to stir 48 hours, and control reaction temperature is at 25 ℃.Product changes with 3000 and carries out centrifugation and (after reaction finishes, carry out centrifugation immediately, in order to avoid SiO
2The colloidal sol conglomeration is assembled), with deionized water ultra-sonic dispersion 1h in ethanol time afterwards that gives a baby a bath on the third day after its birth, obtain the SiO of stable existence in ethanol
2Colloidal sol;
2, be that to dissolve in the 50ml volume percent be in 99.5% the toluene, to make toluene solution for 98.0% vinylbenzene with the 5ml volume percent.Adding 2g mass percent is 99.5% Potassium Persulfate in the 50ml redistilled water, makes initiator solution A; In the 50ml redistilled water, dissolve 0.08g NaHCO in addition
3, make buffered soln B and be used for SiO
2Nano particle is in the dispersion of liquid-liquid interface;
3, the toluene solution that step (2) is made and buffering solution B each 50ml put into beaker and leave standstill 10min to two and be separated, and injecting 2ul content at liquid-liquid interface is the SiO that 6.2g/L step (1) makes
2Colloidal sol.Treat SiO behind the 15min
2Particle is after liquid-liquid interface disperses to finish, and the initiator solution A that 2ml step (2) is made directly injects water, causes the polymerized in-situ reaction.After 24 hours, the film that floats over liquid-liquid interface is shifted out, make and contain SiO
2The particulate polymeric film; Do not add SiO in addition
2Colloidal sol prepares blank polymeric film with identical step;
4. what step (3) is made contains SiO
2SiO is prepared in particulate polymeric film and blank polymeric film compression molding
2The homodisperse polymer composites of nano particle.
The mechanical property of compound back polystyrene has obtained efficient hardening.
Claims (1)
1. utilize liquid-liquid interface to carry out micro-nano granules dispersive method in polymeric matrix, it is characterized in that the steps include:
(1) with the tetraethoxy being main raw material, is ammoniacal liquor, 50-55ml dehydrated alcohol and the mixing of 100ml redistilled water of 25%-28% with the 160-175ml volume percent, stirs 3-10 minute in the constant temperature magnetic stirrer, dropwise adds 18-22ml again with SiO
2The meter volume percent is the tetraethoxy of 20%-30%, continues to stir 5-48 hour, and control reaction temperature is between 12-30 ℃; Product changes with 3000 and carries out centrifugation, after the gained precipitation washing three times in ethanol ultra-sonic dispersion 20-60min, obtain SiO
2Colloidal sol;
(2) the 3-6ml organic monomer is dissolved in 30-60ml and the immiscible organic solvent of water, make organic solution, described organic solvent is a kind of in toluene, benzene and the oil of mirbane, and described organic monomer is a kind of in vinylbenzene and the aniline; Get redistilled water 30-60ml, add 1.5-2.5g organic monomer polymerization starter and make initiator solution A, described organic monomer polymerization starter is a Potassium Persulfate; In the 30-60ml redistilled water, dissolve 0.06-0.10g NaHCO in addition
3Make buffered soln B;
(3) organic solution that equal-volume step (2) is made and buffering solution B are put into beaker and are left standstill 5-10min to two and be separated, and drip the SiO that 2-20ul step (1) makes at liquid-liquid interface
2Colloidal sol; Treat SiO behind the 4-20min
2Particle is after liquid-liquid interface disperses to finish, and the initiator solution A that 1-3mL step (2) is made directly injects water with pipettor, causes the polymerized in-situ reaction; After 24 hours, the composite membrane that floats over liquid-liquid interface is shifted out, make and contain SiO
2The particulate polymeric film; Do not add SiO in addition
2Colloidal sol prepares blank polymeric film with identical step;
What (4) step (3) is made contains SiO
2SiO is prepared in particulate polymeric film and blank polymeric film compression molding
2The homodisperse polymer composites of nano particle.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910113999XA CN101531767B (en) | 2009-04-17 | 2009-04-17 | Micro-nano granules dispersion method in polymer basal body using liquid-liquid interface |
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|---|---|---|---|
| CN200910113999XA CN101531767B (en) | 2009-04-17 | 2009-04-17 | Micro-nano granules dispersion method in polymer basal body using liquid-liquid interface |
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| Publication Number | Publication Date |
|---|---|
| CN101531767A CN101531767A (en) | 2009-09-16 |
| CN101531767B true CN101531767B (en) | 2011-05-18 |
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| CN200910113999XA Expired - Fee Related CN101531767B (en) | 2009-04-17 | 2009-04-17 | Micro-nano granules dispersion method in polymer basal body using liquid-liquid interface |
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| MX2019010615A (en) * | 2017-03-06 | 2019-12-19 | Uti Lp | Device and method of manufacturing a device for detecting hydrocarbons. |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7323540B2 (en) * | 2004-06-16 | 2008-01-29 | North Carolina State University | Process for preparing microrods using liquid-liquid dispersion |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7323540B2 (en) * | 2004-06-16 | 2008-01-29 | North Carolina State University | Process for preparing microrods using liquid-liquid dispersion |
Non-Patent Citations (2)
| Title |
|---|
| Darsh Wasan et al..Colloidal dispersions:Sturcture,stability and geometric confinement.《Powder Technology》.2005,第153卷135-141. * |
| DarshWasanetal..Colloidaldispersions:Sturcture stability and geometric confinement.《Powder Technology》.2005 |
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| CN101531767A (en) | 2009-09-16 |
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