CN101067043A - Polysulfone amide/ZnO nanometer composite material and its prepn process - Google Patents
Polysulfone amide/ZnO nanometer composite material and its prepn process Download PDFInfo
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- CN101067043A CN101067043A CN 200710041151 CN200710041151A CN101067043A CN 101067043 A CN101067043 A CN 101067043A CN 200710041151 CN200710041151 CN 200710041151 CN 200710041151 A CN200710041151 A CN 200710041151A CN 101067043 A CN101067043 A CN 101067043A
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Abstract
The present invention is one kind of polysulfone amide/ZnO nanometer composite material and its preparation process. The composite material consists of aromatic diamine 40-60 wt%, paraphthaloyl chloride 60-40 wt% and nanometer ZnO powder 0.1-5 wt%. The composite material is prepared through a low temperature in-situ polymerization process including the following steps: adding nanometer ZnO powder into N, N-dimethyl acetamide solution via stirring to form dispersed ZnO solution, adding aromatic diamine to form mixed dispersed solution, and adding the other monomer to condensate to form the polysulfone amide/ZnO nanometer composite material. The composite material has the rigidity, size stability and heat resistance of inorganic material and the toughness and machinability of organic material well combined and thus excellent performance.
Description
Technical field
The present invention relates to a kind of polysulfonamides/ZnO nano composite material and preparation method thereof, particularly Polyphenylene Sulfone acid amides/ZnO nano composite material and preparation method thereof.
Background technology
The organic high molecular polymer polysulfonamides is to use engineering plastics more widely, has premium propertiess such as resistance to chemical attack, radiation hardness, high temperature resistant, uninflammability and electrical isolation.Can make good filtering material, also can be used for the insulation paper of motor.Especially be made into textile fibres, more, can be used to make some special spe-cial-purpose uniforms, as antigravity suit, pressure compensating suit, fighting uniform and bunker clothing etc. because it has high-strength, lightweight, resistant to elevated temperatures characteristics.But,, be one of important topic of current material subject so how to improve the over-all properties of polysulfonamides resin because the mechanical property of polysulfonamides does not still satisfy requirement.
How improve on the molecular weight of polymkeric substance in most of doses at the emphasis of research at present, do not see the relevant report that adopts nanotechnology to prepare polysulfonamides and the matrix material of ZnO as yet.
Summary of the invention
One of purpose of the present invention is to provide a kind of polysulfonamides/ZnO nano composite material.
Two of purpose of the present invention is to provide the preparation method of above-mentioned polysulfonamides/ZnO nano composite material.
For achieving the above object, the present invention adopts following technical scheme:
A kind of polysulfonamides/ZnO nano composite material is characterized in that the composition of this matrix material and weight percentage are as follows:
Aromatic diamines 40-60%, p-phthaloyl chloride 60-40%; In addition, press
Above-mentioned raw materials total amount 100% adds nano ZnO powder for benchmark, and its add-on is 0.1-5%;
The size of above-mentioned nano ZnO powder is between 20-50nm.
Above-mentioned aromatic diamines is Ursol D or mphenylenediamine.
Above-mentioned Ursol D is 4 ' 4 diaminodiphenylsulfone(DDS)s; Described mphenylenediamine is 3 ' 3 diaminodiphenylsulfone(DDS)s.
The preparation method of a kind of polysulfonamides according to claim 1/ZnO nano composite material is characterized in that adopting low-temperature in-site polymeric technology, and the processing step of present method is as follows:
A. form and content according to above-mentioned raw material, nano ZnO powder is incorporated in the N,N-dimethylacetamide solvent, high-speed stirring, rotating speed is 12000 rev/mins, stirs 20 minutes, forms the ZnO dispersion soln;
B. aromatic diamines is joined in the above-mentioned ZnO dispersion soln, stir on the limit, the limit dissolving, and be cooled to-8 ℃～-10 ℃; Continue to stir 30 minutes, form the mixed dispersion liquid of nano-ZnO and aromatic diamines.
C. add p-phthaloyl chloride while stirring in the mixed dispersion liquid of nano-ZnO and aromatic diamines, make it carry out polycondensation, the reaction times is 1-1.5 hour, finally forms nano composite material;
D. with the basic solution neutralization, make the pH value of reaction solution reach 6-7, filter then, promptly get product.Described neutralization alkali is calcium chloride or lithium chloride.
When described aromatic diamines was 4 ' 4 diaminodiphenylsulfone(DDS)s or 3 ' 3 diaminodiphenylsulfone(DDS)s, polysulfonamides specifically was expressed as the Polyphenylene Sulfone acid amides.
Among the present invention, typical polysulfonamides is to be formed by diaminodiphenylsulfone(DDS) and p-phthaloyl chloride polycondensation, and its chemical equation is:
The present invention has adopted low-temperature in-site polymeric technology, earlier nano ZnO powder is joined in the N,N-dimethylacetamide solvent, stirs, and forms the ZnO dispersion soln; Then aromatic diamines is joined in the above-mentioned ZnO dispersion soln, form the mixed dispersion liquid of nano-ZnO and aromatic diamines.Last carry out polycondensation with another monomer, make ZnO with the nanoscale homodisperse, be embedded in the polysulfonamides resin, thereby formation polysulfonamides/ZnO nano composite material.This material is with the rigidity of inorganics, and the toughness and the workability of dimensional stability and thermotolerance and organic polymer ideally combine.Can give the many employing traditional methods of material unapproachable premium properties.
The advantage of the inventive method is that technology is simple, and is workable, easy to make and with low cost.
The prepared product of the inventive method is polysulfonamides/ZnO nano composite material, through precipitation bath solidify, operations such as drawing-off, washing, drying, densification, coiling handle, can make polysulfonamides/clay nanocomposites fiber, this is a kind of novel high-performance fiber.
Embodiment
Embodiment one:
A. raw material is prepared: main raw material is 4 ' 4 two amido sulfobenzides, 3 ' 3 two amido sulfobenzides, p-phthaloyl chloride, and nano ZnO powder, its physical size is between 20-50nm.
B. 0.5 gram nano ZnO powder and 300 is restrained the high speed tissue mincer that N ' N---dimethylacetamide solvents are put into a 1000ml, with the rotating speed high speed shear that per minute 12000 changes, the time is 20 minutes, makes it form the nano-ZnO dispersion liquid.
C. above-mentioned suspensoid is poured in the four neck reactors of 500ml, is added 4 ' 4 two amido sulfobenzide and 0.03mol (7.5 gram) 3 ' 3 diaminodiphenylsulfone(DDS)s of 0.09mol (22.35 gram) while stirring, be cooled to-8 ℃---10 ℃; Continue at low temperatures to stir 30 minutes.
D. add the p-phthaloyl chloride of 0.12mol (24.4 gram) in above-mentioned cryogenic fluid while stirring, high-speed stirring makes it carry out polycondensation; React and close cooling pump after 3 minutes, it is heated up naturally.
E. continue reaction after 1 hour, it is 6-7 that the adding calcium oxide is neutralized to pH value; Through filtering discharging, promptly get product at last.
Polymkeric substance is measured the interplanar distance and the transmission electron microscope observation clay layer thickness of the d001 face diffraction peak of material medium clay soil through the X diffraction, show that clay is strutted even dissociated, lamellar spacing only is 20-80nm, be dispersed in the polysulfonamides matrix with nanoscale, the mechanical property of this matrix material sees the following form.
| Conventional polysulfonamides fibre | Polysulfonamides of the present invention/Zn0 nano composite material | |
| Breaking tenacity (cN/dtex) | 2.8-3.0 | 3.5-3.6 |
| Elongation % | 20-25 | 24.95 |
| Degree of crystallinity % | 18 | 27.9 |
| Orientation degree | 69.8 | |
| Heat decomposition temperature | 440.3 | 470 |
Embodiment two:
A. raw material is prepared: main raw material is 4 ' 4 two amido sulfobenzides, p-phthaloyl chloride, and nano ZnO powder, its physical size is between 20-50nm.
B. 0.05 gram nano ZnO powder and 300 is restrained the high speed tissue mincer that N ' N---dimethylacetamide solvents are put into a 1000ml, with the rotating speed high speed shear that per minute 12000 changes, the time is 20 minutes, makes it form the nano-ZnO dispersion liquid.
C. above-mentioned suspensoid is poured in the four neck reactors of 500ml, is added 4 ' 4 two amido sulfobenzides of 30 grams while stirring, be cooled to-8 ℃--10 ℃; Continue at low temperatures to stir 30 minutes.
D. add the p-phthaloyl chloride of 20 grams in above-mentioned cryogenic fluid while stirring, high-speed stirring makes it carry out polycondensation; React and close cooling pump after 3 minutes, it is heated up naturally.
Continue reaction after 1 hour, it is 6--7 that the adding calcium oxide is neutralized to pH value; Through filtering discharging, promptly get product at last.
Embodiment three:
A. raw material is prepared: main raw material is 3 ' 3 two amido sulfobenzides, p-phthaloyl chloride, and nano ZnO powder, its physical size is between 20-50nm.
B. 2.5 gram nano ZnO powders and 300 are restrained the high speed tissue mincer that N ' N---dimethylacetamide solvents are put into a 1000ml, with the rotating speed high speed shear that per minute 12000 changes, the time is 20 minutes, makes it form the nano-ZnO dispersion liquid.
C. above-mentioned suspensoid is poured in the four neck reactors of 500ml, is added 20 grams, 3 ' 3 diaminodiphenylsulfone(DDS)s while stirring, be cooled to-8 ℃--10 ℃; Continue at low temperatures to stir 30 minutes.
D. add the p-phthaloyl chloride of 30 grams in above-mentioned cryogenic fluid while stirring, high-speed stirring makes it carry out polycondensation; React and close cooling pump after 3 minutes, it is heated up naturally.
Continue reaction after 1 hour, it is 6--7 that the adding calcium oxide is neutralized to pH value; Through filtering discharging, promptly get product at last.
Claims (7)
1. polysulfonamides/ZnO nano composite material is characterized in that the composition of this matrix material and weight percentage are as follows:
Aromatic diamines 40-60%, p-phthaloyl chloride 60-40%; In addition, press above-mentioned raw materials total amount 100% and add nano ZnO powder for benchmark, its add-on is 0.1-5%.
2. polysulfonamides according to claim 1/ZnO nano composite material, the size that it is characterized in that the nano ZnO powder that adopts is between 20-50nm.
3. polysulfonamides according to claim 1/ZnO nano composite material is characterized in that described aromatic diamines is one or both in Ursol D, the mphenylenediamine.
4. polysulfonamides according to claim 3/ZnO nano composite material is characterized in that described Ursol D is 4 ' 4 diaminodiphenylsulfone(DDS)s; Described mphenylenediamine is 3 ' 3 diaminodiphenylsulfone(DDS)s.
5. the preparation method of polysulfonamides according to claim 1/ZnO nano composite material is characterized in that adopting low-temperature in-site polymeric technology, and the processing step of present method is as follows:
A. form and content according to above-mentioned raw material, nano ZnO powder is incorporated in the N,N-dimethylacetamide solvent, high-speed stirring, rotating speed is 12000 rev/mins, stirs 20 minutes, forms the ZnO dispersion soln;
B. aromatic diamines is joined in the above-mentioned ZnO dispersion soln, stir on the limit, the limit dissolving, and be cooled to-8 ℃～-10 ℃; Continue to stir 30 minutes, form the mixed dispersion liquid of nano-ZnO and aromatic diamines.
C. add p-phthaloyl chloride while stirring in the mixed dispersion liquid of nano-ZnO and aromatic diamines, make it carry out polycondensation, the reaction times is 1-1.5 hour, finally forms nano composite material;
D. with the basic solution neutralization, make the pH value of reaction solution reach 6-7, filter then, promptly get product.
6. the preparation method of polysulfonamides according to claim 5/ZnO nano composite material is characterized in that described neutralization alkali is calcium chloride or lithium chloride.
7. the preparation method of polysulfonamides according to claim 5/ZnO nano composite material is characterized in that polysulfonamides specifically is expressed as the Polyphenylene Sulfone acid amides when described aromatic diamines is 4 ' 4 diaminodiphenylsulfone(DDS)s or 3 ' 3 diaminodiphenylsulfone(DDS)s.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101457019B (en) * | 2009-01-04 | 2011-06-08 | 上海大学 | Carbon nanotube/polysulfonamide nano composite material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101457019B (en) * | 2009-01-04 | 2011-06-08 | 上海大学 | Carbon nanotube/polysulfonamide nano composite material and preparation method thereof |
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