CN1341667A - Method for initiating polymerization of microemulsion by means of ultrasonic wave - Google Patents
Method for initiating polymerization of microemulsion by means of ultrasonic wave Download PDFInfo
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- CN1341667A CN1341667A CN 00113154 CN00113154A CN1341667A CN 1341667 A CN1341667 A CN 1341667A CN 00113154 CN00113154 CN 00113154 CN 00113154 A CN00113154 A CN 00113154A CN 1341667 A CN1341667 A CN 1341667A
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- ultrasonic wave
- microemulsion
- initiating polymerization
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- monomer
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Abstract
The present invention is characterized by that it utilizes the actions of dispersion, emulsification and initiation of ultrasonic wave to implement microemulsion polymerization under the condition of low temp. and without initiating agent to prepare emulsoid particles with grain size uniformly distributed and grain size of 30 nm-100 nm.
Description
The present invention relates to a kind of method of initiating polymerization of microemulsion by means of ultrasonic wave.
Polymer nano material has extremely important application at aspects such as stealth material, information material, high-performance coating and bio-medical materials.Micro-emulsion polymerization is one of important method of preparation polymer nano-particle, existing more research (1.Larpent C., Bernard E, Richard J., Vaslin S., Macromolecules, 1997,30:354.2 Gan L.M., Chew C.H., Lee K.C., Ng S.C..Polymer, 1993,34:3064.3.Gan L.M., Lee K.C., Chew C.H., NgS.C., Gan L.H..Macromolecules, 1994,27:6335).But there are some limitation in conventional micro-emulsion polymerization, and is big as the emulsifying agent consumption, and emulsifying agent/monomer ratio is greater than 1; Need assistant for emulsifying agent, polymkeric substance purification difficult etc.
Cavitation effect takes place when ultrasonic wave is propagated in liquid medium, promptly in extremely short time and minimum space, produce localized hyperthermia (～5000K), high pressure (～10
8Pa), rate of temperature change reaches 10
9K/s, and be attended by the jet that intensive shockwave and speed per hour reach 400 km.This provides a kind of very special physicochemical environment for chemical reaction.Localized hyperthermia's high pressure that the ultrasonic cavitation effect produces and a series of physics, chemical action are enough to make enter in the cavitation bubble or be positioned near its small molecules cracking produce free radical, thereby cause various chemical reactions.This provides condition for initiating polymerization of microemulsion by means of ultrasonic wave.
The objective of the invention is provides a kind of initiating polymerization of microemulsion by means of ultrasonic wave method at the deficiencies in the prior art, be characterized in utilizing effects such as hyperacoustic dispersion, emulsification, initiation, at lesser temps with need not to realize micro-emulsion polymerization under the situation of initiator, the preparation size distribution is even, and size is at nano level emulsion particle.
The objective of the invention is to realize that by following technical measures wherein said raw material umber is parts by weight except that specified otherwise.
The method of initiating polymerization of microemulsion by means of ultrasonic wave:
(1) 1～40 part of monomer, emulsifying agent 1-10 part, 60～99 parts in dispersion medium and auxiliary agent thereof add in the ultrasound wave irradiation reactor, again with in the ultrasonic wave horn,amplitude transformer insertion reaction device for 0.2～5 part.
(2) fed nitrogen about 2～10 minutes, logical nitrogen speed is 0.1～50 ml/min, and logical circulator bath temperature is 0-50 ℃.
(3) start ultrasonoscope, carry out polyreaction, the ultrasonic power regulation range is at 50-1500w, frequency 2 * 10
4～10
9Hz, 10 minutes～5 hours reaction times.
Monomer is that methyl methacrylate, ethyl propenoate, butyl acrylate, vinylbenzene, vinyl cyanide, acrylamide and/or the vinyl monomer that has surface-active sulfonic acid group, hydroxy-acid group, quaternary ammonium group are at least a.
Emulsifying agent is that sorbitan monooleate, polyoxyethylene (20) Witconol AL 69-66, succsinic acid two-2-ethylhexyl sodium sulfonate, cetyl trimethylammonium bromide, sodium lauryl sulphate, Sodium palmityl sulfate and Sodium dodecylbenzene sulfonate are at least a.
Auxiliary agent is that Polyvinylpyrolidone (PVP), sodium polyacrylate, polyoxyethylene glycol, n-hexyl alcohol, Pentyl alcohol and propyl carbinol are at least a.
Dispersion medium be water and/or with other solvents of water arbitrary proportion blended as alcohol, ketone etc., for the consideration of economy and environment aspect, the most preferred with water.
The emulsion particle median size of the present invention's preparation is 30-100nm, narrow diameter distribution; Polymericular weight is 10
6The order of magnitude.
The present invention has following advantage:
(1) polymerization does not need initiator;
(2) temperature of reaction is lower;
(3) required emulsifier concentration is lower than conventional micro-emulsion polymerization;
(4) particle diameter is little, is nano level and is evenly distributed;
(5) molecular weight of product is higher;
Embodiment:
Below by embodiment the present invention is specifically described.Be necessary to be pointed out that at this following examples only are used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment to the present invention according to the invention described above content.
1. with methyl methacrylate 10g, sodium lauryl sulphate 5g, Pentyl alcohol 1g, water 84g joins in the reactor, feeds about 5 minutes of nitrogen with the oxygen in the eliminating system, and 30 ℃ of control bath temperatures.Open VC-1500 ultrasonic instrument (Sonic﹠amp then; Materials Inc.) beginning polyreaction.Ultrasonic power is 600w in the reaction process, and frequency is 20kHz, and it is constant that nitrogen speed 10 ml/min keep.React and finished in 30 minutes.The polymethylmethacrylate latex particle size of preparation is 36.5nm, and molecular weight is 5.0 * 10
6
2. with butyl acrylate 8g, cetyl trimethylammonium bromide 3g, n-hexyl alcohol 0.5g, water 88.5g joins in the reactor, feeds about 5 minutes of nitrogen with the oxygen in the eliminating system, and 40 ℃ of control bath temperatures.Open VC-1500 ultrasonic instrument (Sonic﹠amp then; Materials Inc.) beginning polyreaction.Ultrasonic power is 200w in the reaction process, and frequency is 40kHz, and it is constant that nitrogen speed 20 ml/min keep.React and finished in 2 hours.The butyl polyacrylate latex particle size of preparation is about 50nm, and molecular weight is 5.5 * 10
6
3. with vinylbenzene 20g, succsinic acid two-2-ethylhexyl sodium sulfonate 4g, Polyvinylpyrolidone (PVP) 0.5g, n-hexyl alcohol 1g, water 74.5g joins in the reactor, feeds about 5 minutes of nitrogen with the oxygen in the eliminating system, and 20 ℃ of control bath temperatures.Open VC-1500 ultrasonic instrument (Sonic﹠amp then; Materials Inc.) beginning polyreaction.Ultrasonic power is 100w in the reaction process, and frequency is 35kHz, and it is constant that nitrogen speed 15 ml/min keep.React and finished in 1 hour.The polystyrene latex grain particle diameter of preparation is about 30nm, and molecular weight is 4.5 * 10
6
Claims (5)
1. the method for initiating polymerization of microemulsion by means of ultrasonic wave is characterized in that:
(1) monomer, 1～40 part, emulsifying agent, 1-10 part, 60～99 parts in dispersion medium and auxiliary agent thereof add in the ultrasound wave irradiation reactor for 0.2～5 part, again with in the ultrasonic wave horn,amplitude transformer insertion reaction device,
(2) fed nitrogen about 2～10 minutes, logical nitrogen speed is 0.1～50 ml/min, and logical circulator bath temperature is 0-50 ℃,
(3) start ultrasonoscope, carry out polyreaction, the ultrasonic power regulation range is at 50-1500w, and frequency is 2 * 10
4～10
9Hz, 10 minutes～5 hours reaction times.
2. according to the method for the described initiating polymerization of microemulsion by means of ultrasonic wave of claim 1, it is characterized in that monomer is that methyl methacrylate, ethyl propenoate, butyl acrylate, vinylbenzene, vinyl cyanide, acrylamide and/or the vinyl monomer that has surface-active sulfonic acid group, hydroxy-acid group, quaternary ammonium group are at least a.
3. according to the method for the described initiating polymerization of microemulsion by means of ultrasonic wave of claim 1, it is characterized in that emulsifying agent is that sorbitan monooleate, polyoxyethylene (20) Witconol AL 69-66, succsinic acid two-2-ethylhexyl sodium sulfonate, cetyl trimethylammonium bromide, sodium lauryl sulphate, Sodium palmityl sulfate and Sodium dodecylbenzene sulfonate are at least a.
4. according to the method for the described initiating polymerization of microemulsion by means of ultrasonic wave of claim 1, it is characterized in that auxiliary agent is that Polyvinylpyrolidone (PVP), sodium polyacrylate, polyoxyethylene glycol, n-hexyl alcohol, Pentyl alcohol and propyl carbinol are at least a.
5. according to the method for the described initiating polymerization of microemulsion by means of ultrasonic wave of claim 1, it is characterized in that dispersion medium be water and/or with water arbitrary proportion blended solvent alcohol and ketone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00113154 CN1118478C (en) | 2000-09-04 | 2000-09-04 | Method for initiating polymerization of microemulsion by means of ultrasonic wave |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00113154 CN1118478C (en) | 2000-09-04 | 2000-09-04 | Method for initiating polymerization of microemulsion by means of ultrasonic wave |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1341667A true CN1341667A (en) | 2002-03-27 |
| CN1118478C CN1118478C (en) | 2003-08-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 00113154 Expired - Lifetime CN1118478C (en) | 2000-09-04 | 2000-09-04 | Method for initiating polymerization of microemulsion by means of ultrasonic wave |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104558322A (en) * | 2013-10-15 | 2015-04-29 | 中国石油化工股份有限公司 | Method for polymerizing acrylamide by ultrasonic technology |
| CN106478883A (en) * | 2016-11-30 | 2017-03-08 | 黄河三角洲京博化工研究院有限公司 | A kind of styrene-butadiene latex and preparation method thereof |
-
2000
- 2000-09-04 CN CN 00113154 patent/CN1118478C/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104558322A (en) * | 2013-10-15 | 2015-04-29 | 中国石油化工股份有限公司 | Method for polymerizing acrylamide by ultrasonic technology |
| CN106478883A (en) * | 2016-11-30 | 2017-03-08 | 黄河三角洲京博化工研究院有限公司 | A kind of styrene-butadiene latex and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1118478C (en) | 2003-08-20 |
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Granted publication date: 20030820 |