CN103642043B - A kind of Trapezoidal ether chain polysilsesquioxane polymer and preparation method thereof - Google Patents
A kind of Trapezoidal ether chain polysilsesquioxane polymer and preparation method thereof Download PDFInfo
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- CN103642043B CN103642043B CN201310536064.9A CN201310536064A CN103642043B CN 103642043 B CN103642043 B CN 103642043B CN 201310536064 A CN201310536064 A CN 201310536064A CN 103642043 B CN103642043 B CN 103642043B
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Abstract
The present invention relates to a kind of Trapezoidal ether chain polysilsesquioxane polymer and preparation method thereof.The technical characteristic preparing a kind of Trapezoidal ether chain polysilsesquioxane polymer is, composition of raw materials: the amount of substance of vinyltrimethoxy silane YDH-171 is 0.05mol, polyoxyethylene glycol PEG
nthe amount of substance of (n=7,13,23 and 33) is 0.06 ~ 0.075mol and ethanol 40ml; Processing condition: catalyzer is sodium hydroxide, solvent is toluene, and temperature is 70 DEG C, and the reaction times is 6 ~ 7h.Beneficial effect is: synthesized a kind of new Trapezoidal ether chain polysilsesquioxane polymer, not only expanded the kind of polysilsesquioxane polymer, and lays the first stone for the application of this base polymer in more wide spectrum.Raw material of the present invention is cheap, and operating procedure is comparatively simple, has certain practical popularization significance.
Description
Technical field
The present invention relates to a kind of Trapezoidal ether chain polysilsesquioxane polymer and preparation method thereof.
Background technology
The application of polysilsesquioxane polymer widely, sums up and mainly makes protective coating, electrically insulating material, adhesives, lithographic resist, dielectric materials and catalystic material etc.Meanwhile, polysilsesquioxane, based on the difference of the Nomenclature Composition and Structure of Complexes, has different outstanding properties, thus is applied in different field.Trapezoidal polysilsesquioxane is one of three kinds of structures the most often existing of this base polymer, there is special rigidity and distinctive duplex structure, chemical property and physical properties has singularity, as good film-forming properties, optical transparence, high thermal stability, mechanical stability, high irradiation stability and high resistance laser threshold etc., the matrix etc. of the macromolecular material of many specific functions, polymer catalyst and optoelectronic information polymer nonlinear optical material can be made.In addition, ether chain group long in polymkeric substance can be given polymer flexibility, hydrophilic oleophobic property, be led the properties such as ionic, and therefore, the polymkeric substance used at some special dimensions is often with long this group of ether chain.Current, based on the thought of polymkeric substance composition, structure design, synthesis Trapezoidal ether chain polysilsesquioxane polymer is the study hotspot of this base polymer of development.
With vinyltrimethoxy silane YDH-171 and polyoxyethylene glycol PEG
n(n=7,13,23 and 33) is monomer, prepares a kind of Trapezoidal ether chain polysilsesquioxane polymer by alcoholysis, polycondensation.The polymkeric substance of this composition, structure will inevitably enrich the kind of polysilsesquioxane polymer, increases the scope of its application.At present, there is not yet any relevant research report.
Summary of the invention
The technical problem solved
In order to expand the Application Areas of polysilsesquioxane polymer, simultaneously also in order to expand this base polymer, the present invention proposes a kind of preparation method of polysilsesquioxane polymer, synthesis obtains a kind of Trapezoidal ether chain polysilsesquioxane polymer.
Technical scheme
The present invention is with vinyltrimethoxy silane YDH-171 and polyoxyethylene glycol PEG
n(n=7,13,23 and 33) is monomer, prepares a kind of polysilsesquioxane polymer by alcoholysis, polycondensation.Its object is to obtain a kind of Trapezoidal ether chain polysilsesquioxane polymer.
A kind of method preparing Trapezoidal ether chain polysilsesquioxane polymer of the present invention, its technical characteristic is:
Synthesizing formula
Vinyltrimethoxy silane YDH-1710.05mol
Polyoxyethylene glycol PEG
n(n=7,13,23 and 33) 0.06 ~ 0.075mol
Ethanol 40ml
Processing condition
Prepare a method for Trapezoidal ether chain polysilsesquioxane polymer, it is characterized in that: concrete steps are as follows:
A) take the vinyltrimethoxy silane YDH-171 of 0.05mol, join in 40ml ethanol and dissolve, then add 0.01mol sodium hydroxide NaOH, proceed in three mouthfuls of reaction flasks after mixing, stir at 70 DEG C;
B) the polyoxyethylene glycol PEG of 0.06 ~ 0.075mol is taken
n(n=7,13,23 and 33), joins stirring and dissolving in the toluene of 200ml under room temperature, in time becoming uniform solution, be slowly transferred in above-mentioned solution;
C) homo(io)thermism stirs 6 ~ 7h, then underpressure distillation at 70 DEG C, obtains colloidal solid;
D) colloidal solid obtained is put into vacuum drying oven, grind into powder after dry 2 days at 100 DEG C, then wash 4 times respectively with sherwood oil and deionized water;
E) put into vacuum drying oven, at 100 DEG C, drying obtains final product in 1 day.
Beneficial effect
The invention has the beneficial effects as follows, provide the synthesis technique that a kind of method is feasible, be easy to realization, synthesis obtains a kind of new Trapezoidal ether chain polysilsesquioxane polymer, this has not only expanded the kind of polysilsesquioxane polymer, and lays the first stone for the application of this base polymer in more wide spectrum.
Accompanying drawing explanation
Fig. 1 is the synthesis process flow diagram of polymkeric substance.
Embodiment
Obtaining Trapezoidal ether chain polysilsesquioxane polymer to synthesize, this invention takes following embodiment:
Take vinyltrimethoxy silane YDH-171 and the 0.01mol sodium hydroxide NaOH of 0.05mol, join in the ethanol of 40ml and dissolve, proceed in three mouthfuls of reaction flasks after mixing, stir at 70 DEG C; Take the polyoxyethylene glycol PEG of 0.06mol
n(n=7,13,23 and 33), joins stirring and dissolving in the toluene of 200ml under room temperature, in time becoming uniform solution, be slowly transferred in above-mentioned solution; Homo(io)thermism stirs 6 ~ 7h, then underpressure distillation at 70 DEG C, obtains colloidal solid; The colloidal solid obtained is put into vacuum drying oven, grind into powder after dry 2 days at 100 DEG C, then wash 4 times respectively with sherwood oil and deionized water; Put into vacuum drying oven, at 100 DEG C, drying obtains final product in 1 day.
Claims (2)
1. a Trapezoidal ether chain polysilsesquioxane polymer, is characterized in that: composition of raw materials: the polyoxyethylene glycol PEG that the amount of substance of vinyltrimethoxy silane YDH-171 is 0.05mol, polymerization degree n is 7,13,23 and 33
namount of substance be 0.06 ~ 0.075mol and ethanol 40ml; Processing condition: catalyzer is sodium hydroxide, solvent is toluene, and temperature is 70 DEG C, and the reaction times is 6 ~ 7h.
2. prepare a method for the Trapezoidal ether chain polysilsesquioxane polymer of claim 1, it is characterized in that: concrete steps are as follows:
A) take the vinyltrimethoxy silane YDH-171 of 0.05mol, join in 40ml ethanol and dissolve, then add 0.01mol sodium hydroxide NaOH, proceed in three mouthfuls of reaction flasks after mixing, stir at 70 DEG C;
B) polymerization degree n taking 0.06 ~ 0.075mol is the polyoxyethylene glycol PEG of 7,13,23 and 33
n, join stirring and dissolving in the toluene of 200ml under room temperature, in time becoming uniform solution, be slowly transferred in above-mentioned solution;
C) homo(io)thermism stirs 6 ~ 7h, then underpressure distillation at 70 DEG C, obtains colloidal solid;
D) colloidal solid obtained is put into vacuum drying oven, grind into powder after dry 2 days at 100 DEG C, then wash 4 times respectively with sherwood oil and deionized water;
E) put into vacuum drying oven, at 100 DEG C, drying obtains final product in 1 day.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310536064.9A CN103642043B (en) | 2013-11-04 | 2013-11-04 | A kind of Trapezoidal ether chain polysilsesquioxane polymer and preparation method thereof |
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| CN201310536064.9A CN103642043B (en) | 2013-11-04 | 2013-11-04 | A kind of Trapezoidal ether chain polysilsesquioxane polymer and preparation method thereof |
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| CN103642043A CN103642043A (en) | 2014-03-19 |
| CN103642043B true CN103642043B (en) | 2016-01-20 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05125191A (en) * | 1991-11-06 | 1993-05-21 | Kanegafuchi Chem Ind Co Ltd | Silicon-based hybrid material |
| WO2005102006A1 (en) * | 2004-04-20 | 2005-11-03 | Dow Corning Corporation | Vesicles of high molecular weight silicone polyethers |
| CN101128515A (en) * | 2005-02-22 | 2008-02-20 | 陶氏康宁公司 | Polyoxyalkylene-alkyl functional siloxane resins and aqueous compositions thereof |
| WO2012060620A2 (en) * | 2010-11-02 | 2012-05-10 | 한국생명공학연구원 | Anti-biofouling ssq/peg network and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2022812B1 (en) * | 2006-05-19 | 2014-04-23 | Dow Corning Toray Co., Ltd. | Polyether-modified organopolysiloxane, diorganopolysiloxane-polyether block copolymer, their production methods, and cosmetic preparation |
| KR20120132164A (en) * | 2011-05-27 | 2012-12-05 | 삼성전자주식회사 | Organic/inorganic hybrid compound for fouling resistance, membrane for fouling resistance, method of preparing membrane for fouling resistance |
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- 2013-11-04 CN CN201310536064.9A patent/CN103642043B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05125191A (en) * | 1991-11-06 | 1993-05-21 | Kanegafuchi Chem Ind Co Ltd | Silicon-based hybrid material |
| WO2005102006A1 (en) * | 2004-04-20 | 2005-11-03 | Dow Corning Corporation | Vesicles of high molecular weight silicone polyethers |
| CN101128515A (en) * | 2005-02-22 | 2008-02-20 | 陶氏康宁公司 | Polyoxyalkylene-alkyl functional siloxane resins and aqueous compositions thereof |
| WO2012060620A2 (en) * | 2010-11-02 | 2012-05-10 | 한국생명공학연구원 | Anti-biofouling ssq/peg network and preparation method thereof |
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