CN101503489A - Preparation of ultra-hydrophobic property polyaniline / polystyrene composite micro-nano material - Google Patents
Preparation of ultra-hydrophobic property polyaniline / polystyrene composite micro-nano material Download PDFInfo
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- CN101503489A CN101503489A CNA2009100246975A CN200910024697A CN101503489A CN 101503489 A CN101503489 A CN 101503489A CN A2009100246975 A CNA2009100246975 A CN A2009100246975A CN 200910024697 A CN200910024697 A CN 200910024697A CN 101503489 A CN101503489 A CN 101503489A
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Abstract
The invention discloses a preparation method of a super-hydrophobic polyaniline/polystyrene composite micro-nano material. The preparation method comprises the following steps: dissolving and dispersing styrene in an aqueous surfactant system, and dropwise adding an initiator to prepare polystyrene nanoparticles with diameter smaller than 100 nanometers; and then adding the polystyrene nanoparticles into a surfactant in which aniline is dissolved and allowing reaction while stirring to obtain the super-hydrophobic polyaniline/polystyrene composite micro-nano material. The preparation method has simple operation, provides obtained polyaniline/polystyrene composite micro-nano tubes with electrical conductivity of polyaniline and toughness of polystyrene as a result of adding the surfactant. And length, width and diameter of the polyaniline/polystyrene composite micro-nano materials can be controlled by adjusting concentration of the surfactant, which provides strong support for fabrication of microelectronic devices.
Description
Technical field
The present invention relates to a kind of preparation technology of hydrophobic polymer material.
Background technology
Polyaniline as a kind of conductive polymers that is widely studied because its unique Doping Mechanism, higher environmental stability, good oxidation-reduction quality and raw material are easy to get etc. feature, exist the potential application prospect at aspects such as solar cell, electromagnetic shielding, molecular device, transmitters.But because difficult processing treatment has then limited the popularization of its practical application.
Summary of the invention
The object of the invention is to invent a kind of polyaniline compound material that is easy to processing treatment---the preparation method of ultra-hydrophobic property polyaniline/polystyrene composite micro-nano material, so that the ultra-hydrophobic property polyaniline/polystyrene composite micro-nano material made of method can be expanded it and becomes and not only conduct electricity but also can be from clean material successively.
The present invention is dissolving dispersion vinylbenzene in the tensio-active agent aqueous systems earlier, drips initiator, and the preparation diameter is less than the polystyrene nanoparticle of 100 nanometers; Then polystyrene nanoparticle is joined in the tensio-active agent that is dissolved with aniline, agitation condition is reaction down, promptly gets ultra-hydrophobic property polyaniline/polystyrene composite micro-nano material.
The present invention is easy and simple to handle, because the adding of tensio-active agent, make made polyaniline/polystyrene composite micro-nano pipe have the electroconductibility of polyaniline, the toughness of polystyrene, adjusting by surfactant concentration simultaneously, may command polyaniline/polystyrene composite micro-nano material length, width and diameter are for the making of microelectronic device provides strong support.
Polyaniline/polystyrene composite micro-nano material with the present invention's preparation utilizes scanning electronic microscope and transmission electron microscope that the product pattern is observed.Measure the molecular structure that gathers the polyaniline/polystyrene mixture by Fourier infrared spectrograph, and x-ray diffractometer is measured the crystallinity of polyaniline/polystyrene mixture.The contact angle of measuring its water and polyaniline/polystyrene material surface by the video contact angle measurement is greater than 130 ° (131 °～156 °), and electroconductibility is good, has the advantages that to be easy to processing treatment from cleaning, is beneficial to further applying of polyaniline.
Preparation diameter of the present invention is during less than the polystyrene nanoparticle of 100 nanometers, vinylbenzene and tensio-active agent are joined in the secondary water, this system was fully stirred 1 hour on magnetic stirring apparatus under 80 ℃ ± 1 ℃ constant temperature, continue in system, to drip initiator under the whipped state, fully reacting 8 hours down in 80 ℃ ± 1 ℃ under the agitation condition again, after reaction finishes, use secondary water, dehydrated alcohol centrifuge washing colourless respectively, product was placed 60 ℃ of vacuum drying ovens 24 hours then to supernatant liquor.
Above-mentioned styrene comprise 5%～20% of the cumulative volume that feeds intake, tensio-active agent amount concentration in cumulative volume is 8～80 mmoles,, secondary water accounts for 60%～91% of the cumulative volume that feeds intake, 2%～5% of the cumulative volume that feeds intake that initiator accounts for.
In addition, aniline, tensio-active agent and polystyrene nanoparticle are joined in the secondary water, after fully stirring 2 hours on the magnetic stirring apparatus, after treating that the solution thorough mixing evenly, ultrasonic again 2 hours, obtain uniform suspension, with this system in 0 ℃ of following constant temperature 1 hour, add initiator solution, stirring mixes system, is positioned over 0 ℃ of following isothermal reaction 24 hours, wait reaction to finish after, use secondary water, dehydrated alcohol centrifuge washing colourless respectively, product was placed 60 ℃ of vacuum drying ovens 24 hours then to supernatant liquor.
Above-mentioned aniline accounts for 0.9%～2% of the cumulative volume that feeds intake, and tensio-active agent amount concentration in cumulative volume is 8～200 mmoles, and polystyrene nanoparticle accounts for 0.09%～1% of the cumulative volume that feeds intake, and initiator solution accounts for 5%～10% of the cumulative volume that feeds intake.
Initiator of the present invention can adopt Diisopropyl azodicarboxylate or ammonium peroxydisulfate or benzoyl peroxide or hydrogen peroxide and blending oxidizing agent.Different initiators feeds intake after can adopting the corresponding solvent dissolving earlier again.
Tensio-active agent of the present invention can adopt Sodium dodecylbenzene sulfonate (SDBS) or sodium lauryl sulphate (SDS) or dialkyl group phenyl ether disulfonic acid or N, N '-two oleoyl quadrol diethyl sodium sulfonates.
Embodiment
Operation steps:
1, diameter is less than the preparation of the polystyrene nanoparticle of 100 nanometers
3～10 milliliters of vinylbenzene and 0.3～0.9 gram tensio-active agent Sodium dodecylbenzene sulfonate (SDBS) are joined in the 50ml secondary water, this system was fully stirred 1 hour on magnetic stirring apparatus under 80 ℃ ± 1 ℃ constant temperature, continue in system, to drip under the whipped state ethanol (less than the 5ml) solution of 0.2～0.6 gram initiator Diisopropyl azodicarboxylate, fully reacting 8 hours down in 80 ℃ ± 1 ℃ under the agitation condition again.Reaction is used centrifugal 3～5 times of secondary water, dehydrated alcohol respectively after finishing, and washs to supernatant liquor colourless.Product was placed 60 ℃ of vacuum drying ovens 24 hours then.
Above-mentioned initiator Diisopropyl azodicarboxylate also can adopt benzoyl peroxide, or hydrogen peroxide and blending oxidizing agent substitute.
2, the preparation of ultra-hydrophobic property polyaniline/polystyrene composite micro-nano material
0.5 gram aniline, 0.3～1.5 gram tensio-active agent Sodium dodecylbenzene sulfonate (SDBS) and above-mentioned reaction gained polystyrene nanoparticle 0.05～0.5 gram are joined in the 50ml secondary water, after fully stirring 2 hours on the magnetic stirring apparatus, after treating that the solution thorough mixing evenly, ultrasonic again 2 hours, obtain uniform suspension.This system in 0 ℃ of following constant temperature 1 hour, is followed disposable adding 5ml initiator ammonium peroxydisulfate saturated aqueous solution, stir system is mixed.Be positioned over 0 ℃ of following isothermal reaction 24 hours.After reaction finishes, use secondary water, dehydrated alcohol centrifuge washing colourless respectively, product was placed 60 ℃ of vacuum drying ovens 24 hours then to supernatant liquor.
The initiator ammonium peroxydisulfate also can adopt Potassium Persulfate or Potassium Iodate to substitute.
Above-mentioned tensio-active agent also can adopt sodium lauryl sulphate (SDS) or dialkyl group phenyl ether disulfonic acid or N, N '-two oleoyl quadrol diethyl sodium sulfonates.
Use:
The ultra-hydrophobic property polyaniline/polystyrene composite micro-nano material that the present invention is prepared utilizes scanning electronic microscope and transmission electron microscope that the product pattern is observed.Measure the molecular structure that gathers the polyaniline/polystyrene mixture by Fourier infrared spectrograph, and x-ray diffractometer is measured the crystallinity of polyaniline/polystyrene mixture.Measure 131 °～156 ° of the contact angles of its water and polyaniline/polystyrene material surface by the video contact angle measurement, electroconductibility is good.
Use example:
1. select SDBS amount of substance concentration 20 mmoles, vinylbenzene is 1 to 1 with the mol ratio of aniline monomer in the polystyrene nanoparticle, and APS is 1 to 1 with the aniline monomer mol ratio, makes the polyaniline/polystyrene micro-nano material.Institute's prepared material is the super-hydrophobic ball of diameter 100-200 nanometer, the video contact angle measurement is measured the contact angle on its water and surface greater than 150 °, roll angle 3-5 °, be scattered in glass surface and find hydrophobic effect, and polyaniline is hydrophilic much larger than polystyrene nanoparticle.Its thermostability is better than polyaniline, has electroconductibility.
2. select SDBS amount of substance concentration 200 mmoles, vinylbenzene is 1 to 10 with the mol ratio of aniline monomer in the polystyrene nanoparticle, and APS is 1 to 1 with the aniline monomer mol ratio, makes the polyaniline/polystyrene micro-nano material.Institute's prepared material is super-hydrophobic rod, the pipe about diameter 100-200 nanometer length 2 μ m, and the video contact angle measurement is measured the contact angle on its water and surface greater than 130 °, and its thermostability is better than polyaniline, has electroconductibility (electroconductibility is higher than super-hydrophobic ball).
Claims (7)
1, the preparation method of ultra-hydrophobic property polyaniline/polystyrene composite micro-nano material is characterized in that dissolving dispersion vinylbenzene in the tensio-active agent aqueous systems earlier, drips initiator, and the preparation diameter is less than the polystyrene nanoparticle of 100 nanometers; Then polystyrene nanoparticle is joined in the tensio-active agent that is dissolved with aniline, agitation condition is reaction down, promptly gets ultra-hydrophobic property polyaniline/polystyrene composite micro-nano material.
2, preparation method according to the described ultra-hydrophobic property polyaniline/polystyrene composite micro-nano material of claim 1, when it is characterized in that described preparation diameter less than the polystyrene nanoparticle of 100 nanometers, vinylbenzene and tensio-active agent are joined in the secondary water, this system was fully stirred 1 hour on magnetic stirring apparatus under 80 ℃ ± 1 ℃ constant temperature, continue in system, to drip initiator under the whipped state, fully reacting 8 hours down in 80 ℃ ± 1 ℃ under the agitation condition again, after reaction finishes, use secondary water respectively, the dehydrated alcohol centrifuge washing is colourless to supernatant liquor, product is placed 60 ℃ of vacuum drying ovens 24 hours then.
3, according to the preparation method of the described ultra-hydrophobic property polyaniline/polystyrene composite micro-nano material of claim 2, it is characterized in that styrene comprise 5%～20% of the cumulative volume that feeds intake, tensio-active agent amount concentration in cumulative volume is 8～80 mmoles, secondary water accounts for 60%～91% of the cumulative volume that feeds intake, 2%～5% of the cumulative volume that feeds intake that initiator accounts for.
4, preparation method according to claim 1 or 2 or 3 described ultra-hydrophobic property polyaniline/polystyrene composite micro-nano materials, it is characterized in that aniline, tensio-active agent and polystyrene nanoparticle join in the secondary water, after fully stirring 2 hours on the magnetic stirring apparatus, after treating that the solution thorough mixing evenly, ultrasonic again 2 hours, obtain uniform suspension, with this system in 0 ℃ of following constant temperature 1 hour, add initiator solution, stirring mixes system, is positioned over 0 ℃ of following isothermal reaction 24 hours, wait reaction to finish after, use secondary water respectively, the dehydrated alcohol centrifuge washing is colourless to supernatant liquor, product is placed 60 ℃ of vacuum drying ovens 24 hours then.
5, according to the preparation method of the described ultra-hydrophobic property polyaniline/polystyrene composite micro-nano material of claim 4, it is characterized in that aniline accounts for 0.9%～2% of the cumulative volume that feeds intake, tensio-active agent amount concentration in cumulative volume is 8～200 mmoles, polystyrene nanoparticle accounts for 0.09%～1% of the cumulative volume that feeds intake, and initiator solution accounts for 5%～10% of the cumulative volume that feeds intake.
6, according to the preparation method of the described ultra-hydrophobic property polyaniline/polystyrene composite micro-nano material of claim 1, it is characterized in that described initiator is Diisopropyl azodicarboxylate or ammonium peroxydisulfate or benzoyl peroxide, or hydrogen peroxide and blending oxidizing agent.
7, according to the preparation method of the described ultra-hydrophobic property polyaniline/polystyrene composite micro-nano material of claim 1; it is characterized in that described tensio-active agent is Sodium dodecylbenzene sulfonate or sodium lauryl sulphate or dialkyl group phenyl ether disulfonic acid or N, N '-two oleoyl quadrol diethyl sodium sulfonates.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798461A (en) * | 2010-03-15 | 2010-08-11 | 厦门大学 | Conductive polymer composite with super hydrophobicity and preparation method thereof |
| CN102093662A (en) * | 2010-12-20 | 2011-06-15 | 昆明理工大学 | ABS resin material with self-cleaned surface and preparation method thereof |
| CN102408664A (en) * | 2011-09-26 | 2012-04-11 | 昆明理工大学 | ABS (acrylonitrile-butadiene-styrene) resin material with surface self-cleaning function and preparation method thereof |
| CN103012823A (en) * | 2012-12-28 | 2013-04-03 | 扬州大学 | Preparation method of bionic compound micro-sphere thin film of polyaniline and polystyrene |
| CN105732861A (en) * | 2014-12-12 | 2016-07-06 | 中国科学院化学研究所 | Polymer hairy sphere, preparation method and application thereof |
| CN113830815A (en) * | 2021-09-24 | 2021-12-24 | 库车塔北泥浆材料有限公司 | Modified barite material and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100478388C (en) * | 2006-11-21 | 2009-04-15 | 南京大学 | Method for preparing conductive, high molecular compound particles of polystyrene / polyaniline |
| CN100588680C (en) * | 2007-12-25 | 2010-02-10 | 北京科技大学 | Method for preparing morphology-controlled polyphenylethene/polyaniline conductive polymeric composite microspheres |
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2009
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798461A (en) * | 2010-03-15 | 2010-08-11 | 厦门大学 | Conductive polymer composite with super hydrophobicity and preparation method thereof |
| CN102093662A (en) * | 2010-12-20 | 2011-06-15 | 昆明理工大学 | ABS resin material with self-cleaned surface and preparation method thereof |
| CN102093662B (en) * | 2010-12-20 | 2013-04-10 | 昆明理工大学 | ABS resin material with self-cleaned surface and preparation method thereof |
| CN102408664A (en) * | 2011-09-26 | 2012-04-11 | 昆明理工大学 | ABS (acrylonitrile-butadiene-styrene) resin material with surface self-cleaning function and preparation method thereof |
| CN103012823A (en) * | 2012-12-28 | 2013-04-03 | 扬州大学 | Preparation method of bionic compound micro-sphere thin film of polyaniline and polystyrene |
| CN105732861A (en) * | 2014-12-12 | 2016-07-06 | 中国科学院化学研究所 | Polymer hairy sphere, preparation method and application thereof |
| CN105732861B (en) * | 2014-12-12 | 2018-09-25 | 中国科学院化学研究所 | Polymer crinosity ball, preparation method and application |
| CN113830815A (en) * | 2021-09-24 | 2021-12-24 | 库车塔北泥浆材料有限公司 | Modified barite material and preparation method thereof |
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