CN101845147A - Method for improving crystallinity of aromatic polysulfonamide using pulsed magnet field - Google Patents
Method for improving crystallinity of aromatic polysulfonamide using pulsed magnet field Download PDFInfo
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- CN101845147A CN101845147A CN 201010126718 CN201010126718A CN101845147A CN 101845147 A CN101845147 A CN 101845147A CN 201010126718 CN201010126718 CN 201010126718 CN 201010126718 A CN201010126718 A CN 201010126718A CN 101845147 A CN101845147 A CN 101845147A
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Abstract
The invention relates to a method for improving crystallinity of aromatic polysulfonamide using a pulsed magnet field. The method comprises the following steps: placing a polysulfonamide film in the pulsed magnet field; controlling magnetic field intensity to be 0.1T-4T and a magnetization period to be 1S-60S; and treating the polysulfonamide film for 5min-300min at the temperature of 20 DEG C to 300 DEG C. Through calculating an XRD spectrogram, the crystallinity of the aromatic polysulfonamide through ultrasonic processing is increased by 10%-35%. The method provides a new idea for improving mechanical properties of the aromatic polysulfonamide and widening application field of the aromatic polysulfonamide, and has a certain innovation and practicality.
Description
Technical field
The present invention relates to a kind of method of improving the polymer crystallization performance, particularly a kind of method of utilizing pulsed magnetic field to improve crystallinity of aromatic polysulfonamide.
Background technology
Experimental results demonstrate that the crystal property of polymkeric substance is except relevant with the regularity of macromolecular chain itself, and is also closely related with external environment condition.These external environment conditions relate generally to temperature, pH, salinity, solvent, electric field, nucleator and other additives etc.Along with the application of magnetics in chemical research, research is subject to people's attention gradually to the polymer crystallization Effect on Performance in relevant magnetic field.People such as Forrest (Forrest B J, Reeves L W.Chem Rev, 1981,81:1～13.) and S.I.Stupp (S.I.Stupp.Pulling polymer into line.Science News.129 (19), 297 (1986)) magnetic field of carrying out liquid crystal polymer and hemihedral crystal macromolecular orientation crystallization influence are studied.(Ning C F such as Ning Chaofeng, Li G Y, Hu C P.China Synthetic RubberIndustry.2000,23 (5): 320-321) exist the form of the polyurethane elastomer for preparing down to study to magnetic field, be respectively 1.5T, 1.0T and do not exist in magneticstrength and synthesized hard section massfraction under the situation of magnetic field and be 50% polyurethane elastomer, characterized their form with WAXD and SEM.The result shows: magnetic field exists the degree of crystallinity of the polyurethane elastomer for preparing down obviously to increase, and magneticstrength is strong more, and degree of crystallinity is big more.It is feasible that these researchs show that all the method for utilizing magnetic field to improve the polymer crystallization performance is undoubtedly.
Polysulfonamides (PSA) fiber has been filled up the blank of China's heat-resistance and flame-retardant fiber with its good thermotolerance, thermostability, high temperature dimensional stability, flame retardant resistance, electrical insulating property and radioresistance, it is the material of following a very long time China's focus development, the shortcoming that but the crystallization rate of polysulfonamides own is slow, degree of crystallinity is low has influenced its mechanical property to a certain extent, thereby has contained that it is in the high-performance fiber Application for Field.And at present about improving modification and the blend aspect that its crystalline method mostly concentrates on polysulfonamides itself, Tang Zhi bravely waits (Liu Jiexia, Tang Zhiyong, Sun Jinliang. the preparation of polysulfonamides nano composite material and fiber thereof and sign [J]. industry textile product .2007 (2): 14-20) with polysulfonamides and the compound preparation PSA/ZnO of inorganic powder nano composite material, the degree of crystallinity and the mechanical property of polysulfonamides have been improved to a certain extent, but the scattering problem about nanoparticle is not well solved, and can not realize industrialized production.People such as M.D.Guiver (Michael D.Guiverand Gilles P.Robertson.Chemical Modification of Polysulfones:A Facile Method ofPreparingAzide Derivatives from Lithiated PolysulfoneIntermediates[J] .Macromolecules 1995,28,294-301) utilize the method for chemical modification to change the chemical structure of polysulfonamides, mechanical property is improved, but in the monomer preparation process, need to have reduced productive rate through the multistep organic reaction.As seen utilize the modification of polysulfonamides own to improve its degree of crystallinity certain limitation is arranged, the present invention is in conjunction with above-mentioned research about external field evoked polymer crystallization, proposition utilizes pulsed magnetic field to improve the imagination of crystallinity of aromatic polysulfonamide, for the range of application of expanding polysulfonamides fibre has proposed new thinking, certain theoretical investigation value and market using value are arranged.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing pulsed magnetic field to improve crystallinity of aromatic polysulfonamide.
The present invention utilizes pulsed magnetic field that polysulfonamides is handled based on the magnetic field theory that reconstruct is built to macromolecular conformation, to improve the crystal property of polysulfonamides, remedies that the polysulfonamides fibre crystallization rate is slow now, degree of crystallinity is low, the shortcoming of poor mechanical property.Ultimate principle of the present invention is: magnetic field comes from the effect of the magnetizing force that material is subjected to the influence of polymer crystallization in magnetic field, polymer segment has improved its motor capacity owing to be subjected to the effect of magnetizing force, improves its crystal property.In addition, magnetic field must also influence macromolecular conformation to the influence that reaches the interaction (comprising hydrogen bond action, hydrophobic interaction, electrostatic interaction and Van der Waals force etc.) between macromole in the macromole, high molecular aggregated structure is constructed again, thereby influenced high molecular crystal property.
According to above-mentioned principle, the present invention adopts following technical scheme:
A kind of method of utilizing pulsed magnetic field to improve crystallinity of aromatic polysulfonamide, the concrete steps that it is characterized in that this method are: the polysulfonamides film is placed pulsed magnetic field, controlling magnetic field intensity is 0.1T～4T, the cycle of magnetizing is 1S～60S, under 20 ℃～300 ℃ temperature, handle 5min～300min.
The thickness of above-mentioned polysulfonamides film is 0.01mm～0.5mm.
A kind of method of utilizing pulsed magnetic field to improve crystallinity of aromatic polysulfonamide, the concrete steps that it is characterized in that this method are: polysulfonamides fibre is placed pulsed magnetic field, controlling magnetic field intensity is 0.1T～4T, the cycle of magnetizing is 1S～60S, handles 5min～100min under 210 ℃～300 ℃ temperature.
The diameter of above-mentioned polysulfonamides fibre is 0.1mm～1.0mm.
Through the polysulfonamides that the pulse magnetic field treatment is crossed, its degree of crystallinity is significantly improved, and degree of crystallinity has improved 10%～35%, has improved the mechanical property of polysulfonamides.The inventive method has been expanded the range of application of polysulfonamides fibre, has certain theoretical investigation value and market using value.
Description of drawings:
Fig. 1 is the polysulfonamides film XRD comparison diagram that has or not pulsed magnetic field to handle under 50 ℃, wherein a is the no pulse magnetic field treatment, be embodiment 1 pairing polysulfonamides film XRD figure, b is that magneticstrength is under the pulsed magnetic field processing of 1T, i.e. embodiment 4 pairing polysulfonamides film XRD figure.
Fig. 2 is the polysulfonamides film XRD comparison diagram that has or not pulsed magnetic field to handle under 270 ℃, wherein c is the no pulse magnetic field treatment, be embodiment 3 pairing polysulfonamides film XRD figure, d is that magneticstrength is under the pulsed magnetic field processing of 1T, i.e. embodiment 8 pairing polysulfonamides film XRD figure.
Fig. 3 is the polysulfonamides fibre XRD comparison diagram that has or not pulsed magnetic field to handle under 270 ℃, wherein e is the no pulse magnetic field treatment, be embodiment 9 pairing polysulfonamides fibre XRD figure, f is that magneticstrength is under the pulsed magnetic field processing of 1T, i.e. embodiment 10 pairing polysulfonamides fibre XRD figure.
Embodiment
Describe the present invention below in conjunction with embodiment.
The configuration quality mark is polysulfonamides (PSA)-N of 16%, N dimethyl hexanamide (DMAc) solution, adopt the method for solution film forming to prepare the polysulfonamides film on cover glass, choosing thickness by sieve method is that polysulfonamides film about 0.1mm is some stand-by.
The configuration quality mark is polysulfonamides (PSA)-N of 16%, and N dimethyl hexanamide (DMAc) solution adopts the method for wet-spinning to prepare polysulfonamides fibre, and choosing diameter by sieve method is that polysulfonamides fibre about 0.5mm is some stand-by.
Embodiment 1: 1 of polysulfonamides film getting embodiment 1 preparation places 50 ℃ air dry oven to heat-treat, treatment time is 2h, after processing finishes film is washed to remove solvent, polymer segment is freezed, utilize the crystal property of sample after the XRD characterization process.
Embodiment 2: present embodiment is substantially the same manner as Example 1, and different is: heat treated temperature is set to 160 ℃, and the treatment time is 1h.Utilize the crystal property of sample after the XRD characterization process.
Embodiment 3: present embodiment is substantially the same manner as Example 1, and different is: heat treated temperature is set to 270 ℃, and the treatment time is 15min.Utilize the crystal property of sample after the XRD characterization process.
Embodiment 4: getting 1 of polysulfonamides film, to place magneticstrength be 1T, and the cycle of magnetizing is to handle in the pulsed magnetic field of 15S, and to utilize temperature regulating device control sample temperature be 50 ℃, and the treatment time is 2h.Utilize the crystal property of sample after the XRD characterization process.
Embodiment 5: present embodiment is substantially the same manner as Example 4, and different is: magneticstrength is set to 2T.
Embodiment 6: present embodiment is substantially the same manner as Example 4, and different is: magneticstrength is set to 4T.
Embodiment 7: present embodiment is substantially the same manner as Example 4, and different is: temperature is set to 160 ℃, and the treatment time is 1h.
Embodiment 8: present embodiment is substantially the same manner as Example 4, and different is: temperature is set to 270 ℃, and the treatment time is 15min.
Embodiment 9: get 15 of polysulfonamides fibres (length is 10cm) marshalling, place 270 ℃ air dry oven to heat-treat, the treatment time is 15min.Utilize the crystal property of fiber after the XRD characterization process.
Embodiment 10: get 15 of polysulfonamides fibres (length is 10cm) marshalling, placing magneticstrength is 1T, and the cycle of magnetizing is to handle in the pulsed magnetic field of 15S, and to utilize temperature regulating device control sample temperature be 270 ℃, and the treatment time is 15min.Utilize the crystal property of fiber after the XRD characterization process.
Embodiment 11: this enforcement is substantially the same manner as Example 10, and different is: magneticstrength is set to 2T.
Embodiment 12: this enforcement is substantially the same manner as Example 10, and different is: magneticstrength is set to 4T.
By the above-mentioned embodiment contrast that has or not pulsed magnetic field, in conjunction with Fig. 1 and Fig. 2, can find, for polysulfonamides, no matter be its solution crystallization process in the time of 50 ℃～160 ℃, still near the crystallisation process of (240 ℃～270 ℃) its second-order transition temperature applies pulsed magnetic field and all can produce active influence to its crystallisation process, improve the crystal property of polysulfonamides, improve its degree of crystallinity.After applying pulsed magnetic field by scaling system 1, Fig. 2 and Fig. 3, the degree of crystallinity of polysulfonamides film has improved 14.3% and 18.5% respectively, and the degree of crystallinity of polysulfonamides acid amides has improved 23.7%.Above-mentioned description to example is can understand and apply the invention for the ease of those skilled in the art.Those of ordinary skill in the art can be easy to these embodiments are made various modifications, and needn't pass through performing creative labour being applied in the general principle of this explanation in other application example.Therefore, the invention is not restricted to the embodiment here, those skilled in the art should be within protection scope of the present invention to improvement and modification that the present invention makes according to announcement of the present invention.
Claims (4)
1. method of utilizing pulsed magnetic field to improve crystallinity of aromatic polysulfonamide, the concrete steps that it is characterized in that this method are: the polysulfonamides film is placed pulsed magnetic field, controlling magnetic field intensity is 0.1T～4T, the cycle of magnetizing is 1S～60S, under 20 ℃～300 ℃ temperature, handle 5min～300min.
2. according to the described method of utilizing pulsed magnetic field to improve crystallinity of aromatic polysulfonamide of claim, the thickness that it is characterized in that described polysulfonamides film is 0.01mm～0.5mm.
3. method of utilizing pulsed magnetic field to improve crystallinity of aromatic polysulfonamide, the concrete steps that it is characterized in that this method are: polysulfonamides fibre is placed pulsed magnetic field, controlling magnetic field intensity is 0.1T～4T, the cycle of magnetizing is 1S～60S, handles 5min～100min under 210 ℃～300 ℃ temperature.
4. according to the described method of utilizing pulsed magnetic field to improve crystallinity of aromatic polysulfonamide of claim, the diameter that it is characterized in that described polysulfonamides fibre is 0.1mm～1.0mm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172604A (en) * | 2011-12-22 | 2013-06-26 | 北大方正集团有限公司 | Lovastatin purification method combining auxiliary magnetic crystallization |
| CN104790051A (en) * | 2015-04-14 | 2015-07-22 | 上海大学 | Nylon 6 melt spinning method and device under external field condition |
| CN104831384A (en) * | 2015-04-14 | 2015-08-12 | 上海大学 | Melt spinning method with application of regulating pulsed magnetic field and melt spinning apparatus |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101088594A (en) * | 2007-07-11 | 2007-12-19 | 湖北工业大学 | Process of preparing tubular porous membrane with high permeating flux |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101088594A (en) * | 2007-07-11 | 2007-12-19 | 湖北工业大学 | Process of preparing tubular porous membrane with high permeating flux |
Non-Patent Citations (1)
| Title |
|---|
| 《化工新型材料》 19861231 陈贻瑞 等 磁场效应在高聚物领域中的应用 第1-5页 1-4 , 第7期 2 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172604A (en) * | 2011-12-22 | 2013-06-26 | 北大方正集团有限公司 | Lovastatin purification method combining auxiliary magnetic crystallization |
| CN103172604B (en) * | 2011-12-22 | 2015-06-24 | 北大方正集团有限公司 | Lovastatin purification method combining auxiliary magnetic crystallization |
| CN104790051A (en) * | 2015-04-14 | 2015-07-22 | 上海大学 | Nylon 6 melt spinning method and device under external field condition |
| CN104831384A (en) * | 2015-04-14 | 2015-08-12 | 上海大学 | Melt spinning method with application of regulating pulsed magnetic field and melt spinning apparatus |
| CN104790051B (en) * | 2015-04-14 | 2017-05-31 | 上海大学 | The melt-spinning method of nylon 6 and melt-spinning apparatus under condition of external field |
| CN104831384B (en) * | 2015-04-14 | 2017-06-23 | 上海大学 | Apply the method and melt-spinning apparatus of the melt spinning in pulse regulatable magnetic field |
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Open date: 20100929 |