CN102337606B - A polyaryl sulfone amide spinning solution with a high nozzle draw ratio and its preparation method - Google Patents
A polyaryl sulfone amide spinning solution with a high nozzle draw ratio and its preparation method Download PDFInfo
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Abstract
The invention relates to an aromatic polysulfonamide spinning solution with high-power jet stretch ratio and a preparation method thereof. The mass fraction of aromatic polysulfonamide in the spinning solution is 5 to 35 percent, the apparent viscosity of the solution is 20 to 1000 Pa.s at the temperature being 90 DEG C, and the jet stretch ratio of the spinning solution is 2 to 10. The preparation process comprises the steps that: the aromatic polysulfonamide is mixed with solvents, the mixed swelling is carried out for 0.5 to 1h at the temperature being 20 to 75 DEG C, and transparent, uniform and stable spinning solution is obtained through kneading dissolving. The spinning solution prepared by the preparation method has the advantages that the apparent viscosity is great, the relaxation time is long, a dry-jet wet-spinning method can be adopted for spinning, the greater jet stretch ratio and the higher spinning velocity are adopted, the yield is improved, the orientation of aromatic polysulfonamide macromolecules after spinning solution extrusion is fully ensured, the orientation and the crystallization in the after-stretching and heat treatment processes are favorably realized, and the mechanical property of fibers is favorably improved.
Description
Technical field
The present invention relates to a kind of aromatic polysulfonamide spinning solution with high power jet stretch ratio and preparation method thereof.
Background technology
The aromatic polysulfonamide fiber be a kind of industry with and special protection with being main heat resistance fiber, be a kind of can the use for a long time more than 250 ℃, the fiber that perhaps under higher temperature, can use moment.
The aromatic polysulfonamide fiber has superior heat resistance, good electrical insulating property, good DIMENSIONAL STABILITY and chemical resistance, exposure at high temperature still can keep good physical property, it is at the high temperature filtration bag, heatproof fireproof garment and F.H level electrically-insulating paper and some other industrial application.
The preparation method of preparation aromatic polysulfonamide fiber is wet spinning at present, wherein the preparation method of spinning solution mostly is: with 4,4 '-diamino diphenyl sulfone (4,4 '-DDS), 3,3 '-diamino diphenyl sulfone (3,3 '-DDS) dissolves in amide solvent, after adding paraphthaloyl chloride (TPC) low temperature polymerization, with the spinning solution that obtains certain solid content in the inorganic base with the HCl that generates.
Chinese patent CN101275308A disclose a kind of complete between among the preparation method of position aromatic polysulfonamide fiber the preparation process of its spinning solution be: with 3,3 '-diamino-diphenyl sulfone is dissolved in the organic solvent and is cooled to-20～20 ℃, add and 3 again, low temperature polymerization behind the paraphthaloyl chloride of 3 '-diamino-diphenyl sulfone equimolar amounts, with in the inorganic base and the hydrogen chloride that generates, make the spinning solution that solid content is 10wt%～20wt%.
The preparation method that Chinese patent CN1389604 discloses spinning solution among a kind of preparation method of polysulfonamides fibre is as follows: in varing proportions 4,4 '-diamino diphenyl sulfone (4,4 '-DDS), 3,3 '-diamino diphenyl sulfone (3,3 '-DDS) dissolves in amide solvent, be cooled to low temperature-20～5 ℃ lower with paraphthaloyl chloride (TPC) polymerization after, with obtaining the spinning solution that solid content is 10wt%～20wt% with the HCl that generates in the inorganic base.
Chinese patent CN1264896C discloses the method for continuous double-screw preparation of polysulfone amide solution, with 4 of certain proportioning, 4 '-diamino diphenyl sulfone (4,4 '-DDS), 3,3 '-diamino diphenyl sulfone (3,3 '-DDS) is dissolved in the amide solvent, add a certain proportion of graininess or molten state paraphthaloyl chloride (TPC) after the cooling through pre-polymerization or without pre-polymerization, then enter in the double screw extruder, reacted 10～25 minutes, and generated containing hydrogen chloride polysulfonamides solution.With calcium hydroxide or calcium oxide neutralization hydrogen chloride wherein, its solid content of polysulfonamides solution that obtains being directly used in spinning is 12wt%～20wt%, than dense logarithm viscosity number more than 1.4.
Chinese patent CN101255231A has announced a kind of method of preparing polysulfonamides polymeric solution by segment polymerization, the method is by 4 of mass fraction 10: 90～90: 10,4 '-diamino diphenyl sulfone (4,4 '-DDS), 3,3 '-diamino diphenyl sulfone (3,3 '-DDS) is dissolved in the cooler in organic solvent and is cooled to-10～10 ℃, preparing solid content by continous mode precondensation and batch (-type) polycondensation polymerization is 1～20wt%, and logarithmic viscosity number is the polysulfonamides solution more than 2.0.
The preparation process that Chinese patent 101718002A discloses its spinning solution in a kind of preparation of ultrafine polysulfonainide fiber is: prepare the aromatic polysulfonamide master batch with conventional method, master batch is dissolved in the intensive polar solvent, obtain solid content and be 11～25% spinning solution, be directly used in the wet spinning under the electric field action.
The spinning solution of said method element preparation all is used for wet spinning, there are the characteristics that solution viscosity is low, jet stretch ratio is little, be unfavorable for the macromolecular orientation in the as-spun fibre, in a single day fiber solidifies, because of stronger interactions such as intermolecular hydrogen bondings, macromolecular orientation structure in the postorder drawing process is difficult to form, and causes fibre crystallinity, and fibrous mechanical property is relatively poor.The main cause that the spinning solution jet stretch ratio is little is that the solution apparent viscosity is low, and slack time is short, and the orientation that solution produces after spinneret orifice is extruded is very fast lax, and extruding strand, can to bear on the spinning threadling ability of tension force little.
Summary of the invention
The purpose of this invention is to provide a kind of aromatic polysulfonamide spinning solution with high power jet stretch ratio and preparation method thereof, be intended to solve prior art spinning solution slack time short so that orientation that solution produces and relax, extrude strand and can bear the little problem of the ability of tension force on the spinning threadling very soon after spinneret orifice is extruded.
A kind of aromatic polysulfonamide spinning solution with high power jet stretch ratio of the present invention, the mass fraction of aromatic polysulfonamide is 5～35% in the described spinning solution, is 20～1000Pas in the apparent viscosity of 90 ℃ of lower solution of temperature; The jet stretch ratio of described spinning solution is 2～10, namely enters the first coagulating bath at spinning solution after spinneret orifice is extruded, and the drafting rate that goes out the first coagulating bath is 2～10 with the ratio of the speed that spinneret orifice is extruded.
As preferred technical scheme:
Aforesaid a kind of aromatic polysulfonamide spinning solution with high power jet stretch ratio, the solvent of described spinning solution viscosity at normal temperatures is greater than 0.01Pas, a kind of in 1-butyl-3-methylimidazole villaumite, 1-butyl-3-methylimidazole bromine salt, 1-allyl-3-methylimidazole bromine salt, 1-ethyl-3 methylimidazole acetate, 1-ethyl-3 methylimidazole formates or the 1-ethyl-3 methylimidazole methyl phosphite salt.
Aforesaid a kind of aromatic polysulfonamide spinning solution with high power jet stretch ratio, described aromatic polysulfonamide are the homopolymers that is comprised of a kind of construction unit in structural formula (1)～(4) or by any two kinds of random copolymers that construction unit forms in structural formula (1)～(4);
Structural formula (1)
Structural formula (2)
Structural formula (3)
Structural formula (4)
The weight average molecular weight of described aromatic polysulfonamide is 10000～1000000.
Two kinds of construction unit molar ratios of the random copolymerization aromatic polysulfonamide that described any two kinds of construction units form are 1: 9～9: 1.
Described spinning temperature is 70～160 ℃.
Described spinneret orifice draw ratio is 1～2, can preferred 1.5.
Described the first coagulation bath composition is 30～60wt% solvent and excess water, preferred 40wt% solvent and excess water; Temperature-10～40 ℃, preferred 10 ℃.
The speed that described spinning solution goes out spinneret orifice is 1～40m/min, preferred 10m/min.
After described spinning solution goes out spinneret orifice, enter coagulating bath before, one section air layer can be set, the length of air layer is 0～80mmm, preferred 40mm.
The present invention also provides a kind of preparation method with aromatic polysulfonamide spinning solution of high power jet stretch ratio, aromatic polysulfonamide is mixed with the mass ratio of solvent according to 5: 95～35: 65, at 20～75 ℃ of lower swelling 0.5～1h that mix of temperature, mediate the spinning solution that dissolving obtains transparent stable homogeneous at 70～160 ℃, described spinning solution is 20～1000Pas in the apparent viscosity of 90 ℃ of lower solution of temperature.
Aforesaid a kind of preparation method with aromatic polysulfonamide spinning solution of high power jet stretch ratio, described aromatic polysulfonamide is the homopolymers that is comprised of a kind of construction unit in structural formula (1)～(4) or by any two kinds of random copolymers that construction unit forms in structural formula (1)～(4);
Structural formula (1)
Structural formula (2)
Structural formula (3)
Structural formula (4)
The weight average molecular weight of described aromatic polysulfonamide is 10000～1000000.
Two kinds of construction unit molar ratios of the random copolymerization aromatic polysulfonamide that described any two kinds of construction units form are 1: 9～9: 1.
Aforesaid a kind of preparation method with aromatic polysulfonamide spinning solution of high power jet stretch ratio, the solvent of described spinning solution viscosity at normal temperatures is greater than 0.01Pas, a kind of in 1-butyl-3-methylimidazole villaumite, 1-butyl-3-methylimidazole bromine salt, 1-allyl-3-methylimidazole bromine salt, 1-ethyl-3 methylimidazole acetate, 1-ethyl-3 methylimidazole formates or the 1-ethyl-3 methylimidazole methyl phosphite salt.
Beneficial effect:
A kind of aromatic polysulfonamide spinning solution with high power jet stretch ratio of the present invention and preparation method thereof, the solution apparent viscosity is large, and slack time is large, can adopt the method for dry-jet wet-spinning to carry out spinning, adopt larger shower nozzle draw ratio and spinning speed, productive rate improves; Confiscating guarantees that spinning solution extrudes the macromolecular orientation of rear aromatic polysulfonamide, is conducive to orientation and crystallization in after-drawing, the heat treatment process, is conducive to improve fibrous mechanical property.
The specific embodiment
Below in conjunction with the specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
A kind of aromatic polysulfonamide spinning solution with high power jet stretch ratio of the present invention, the mass fraction of aromatic polysulfonamide is 5～35% in the described spinning solution, is 20～1000Pas in the apparent viscosity of 90 ℃ of lower solution of temperature; The spinneret draft ratio of described spinning solution is 2～10, and namely spinning solution enters the first coagulating bath after spinneret orifice is extruded, and the drafting rate that goes out the first coagulating bath is 2～10 with the ratio of the speed that spinneret orifice is extruded.
Aforesaid a kind of aromatic polysulfonamide spinning solution with high power jet stretch ratio, described aromatic polysulfonamide are the homopolymers that is comprised of a kind of construction unit in structural formula (1)～(4) or by any two kinds of random copolymers that construction unit forms in structural formula (1)～(4);
Structural formula (1)
Structural formula (2)
Structural formula (3)
Structural formula (4)
The weight average molecular weight of described aromatic polysulfonamide is 10000～1000000.
Two kinds of construction unit molar ratios of the random copolymerization aromatic polysulfonamide that described any two kinds of construction units form are 1: 9～9: 1.
Aforesaid a kind of aromatic polysulfonamide spinning solution with high power jet stretch ratio, the solvent of described spinning solution viscosity at normal temperatures is greater than 0.01Pas, a kind of in 1-butyl-3-methylimidazole villaumite, 1-butyl-3-methylimidazole bromine salt, 1-allyl-3-methylimidazole bromine salt, 1-ethyl-3 methylimidazole acetate, 1-ethyl-3 methylimidazole formates or the 1-ethyl-3 methylimidazole methyl phosphite salt.
Embodiment 1
With weight average molecular weight be 10000, the aromatic polysulfonamide that is comprised of the unit in the structural formula (1) mixes according to 5: 95 mass ratio with solvent 1-butyl-3-methylimidazole villaumite, at 75 ℃ of lower swelling 0.5h that mix of temperature, under 70 ℃, mediate dissolving 100h, obtain the spinning solution of transparent stable homogeneous.Described spinning solution is 20Pas in the apparent viscosity of 90 ℃ of lower solution of temperature.
Spinning solution enters the first coagulating bath after spinneret orifice is extruded, the drafting rate that goes out the first coagulating bath is 2 with the ratio of the speed that spinneret orifice is extruded.Described spinning temperature is 70 ℃, described spinneret orifice draw ratio is 1.5, described the first coagulation bath composition is 5 ℃ of 60wt% solvent and excess water, temperature, and the speed that spinning solution goes out spinneret orifice is 20m/min, and the air gap length of described spinning solution from the spinneret orifice to the coagulating bath is 10mm.
Embodiment 2
The aromatic polysulfonamide that weight average molecular weight is 1000000, unit in the structural formula (2) forms is mixed with the mass ratio of solvent 1-ethyl-3 methylimidazole methyl phosphite salt according to 35: 65, at 20 ℃ of lower swelling 1h that mix of temperature, under 160 ℃, mediate dissolving 50h, obtain the spinning solution of transparent stable homogeneous.Described spinning solution is 1000Pas in the apparent viscosity of 90 ℃ of lower solution of temperature.
Spinning solution enters the first coagulating bath after spinneret orifice is extruded, the drafting rate that goes out the first coagulating bath is 10 with the ratio of the speed that spinneret orifice is extruded.Described spinning temperature is 160 ℃, described spinneret orifice draw ratio is 1.5, described the first coagulation bath composition is 10 ℃ of 30wt% solvent and excess water, temperature, and the speed that spinning solution goes out spinneret orifice is 5m/min, and the air gap length of described spinning solution from the spinneret orifice to the coagulating bath is 80mm.
Embodiment 3
With weight average molecular weight be 100000, structural formula (1) mixes with the mass ratio of solvent solvent 1-ethyl-3 methylimidazole methyl phosphite salt according to 10: 90 with the aromatic polysulfonamide that unit (molar ratio is 1: 9) in the structural formula (2) forms, at 40 ℃ of lower swelling 1h that mix of temperature, under 100 ℃, mediate dissolving 72h, obtain the spinning solution of transparent stable homogeneous.Described spinning solution is 80Pas in the apparent viscosity of 90 ℃ of lower solution of temperature.
Spinning solution enters the first coagulating bath after spinneret orifice is extruded, the drafting rate that goes out the first coagulating bath is 6 with the ratio of the speed that spinneret orifice is extruded.Described spinning temperature is 100 ℃, described spinneret orifice draw ratio is 1.5, described the first coagulation bath composition is 40 ℃ of 50wt% solvent and excess water, temperature, and the speed that spinning solution goes out spinneret orifice is 15m/min, and the air gap length of described spinning solution from the spinneret orifice to the coagulating bath is 50mm.
Embodiment 4
With weight average molecular weight be 200000, structural formula (3) mixes according to 15: 85 mass ratio with solvent 1-allyl-3-methylimidazole bromine salt with the aromatic polysulfonamide that unit (molar ratio is 9: 1) in the structural formula (4) forms, under temperature 50 C, mix swelling 1h, under 110 ℃, mediate dissolving 48h, obtain the spinning solution of transparent stable homogeneous.Described spinning solution is 150Pas in the apparent viscosity of 90 ℃ of lower solution of temperature.
Spinning solution enters the first coagulating bath after spinneret orifice is extruded, the drafting rate that goes out the first coagulating bath is 7 with the ratio of the speed that spinneret orifice is extruded.Described spinning temperature is 110 ℃, described spinneret orifice draw ratio is 1.5, described the first coagulation bath composition is 30 ℃ of 45wt% solvent and excess water, temperature, and the speed that spinning solution goes out spinneret orifice is 12m/min, and the air gap length of described spinning solution from the spinneret orifice to the coagulating bath is 40mm.
Embodiment 5
With weight average molecular weight be 150000, structural formula (1) mixes with the mass ratio of solvent 1-ethyl-3 methylimidazole acetate according to 20: 80 with the aromatic polysulfonamide that unit (molar ratio is 1: 2) in the structural formula (4) forms, under temperature 45 C, mix swelling 1h, under 110 ℃, mediate dissolving 48h, obtain the spinning solution of transparent stable homogeneous.Described spinning solution is 250Pas in the apparent viscosity of 90 ℃ of lower solution of temperature.
Spinning solution enters the first coagulating bath after spinneret orifice is extruded, the drafting rate that goes out the first coagulating bath is 6.5 with the ratio of the speed that spinneret orifice is extruded.Described spinning temperature is 110 ℃, described spinneret orifice draw ratio is 1.5, described the first coagulation bath composition is 12 ℃ of 40wt% solvent and excess water, temperature, and the speed that spinning solution goes out spinneret orifice is 10m/min, and the air gap length of described spinning solution from the spinneret orifice to the coagulating bath is 40mm.
Embodiment 6
With weight average molecular weight be 120000, structural formula (2) mixes with the mass ratio of solvent 1-ethyl-3 methylimidazole formates according to 25: 75 with the aromatic polysulfonamide that unit (molar ratio is 2: 1) in the structural formula (3) forms, under temperature 60 C, mix swelling 0.5h, under 120 ℃, mediate dissolving 45h, obtain the spinning solution of transparent stable homogeneous.Described spinning solution is 450Pas in the apparent viscosity of 90 ℃ of lower solution of temperature.
Spinning solution enters the first coagulating bath after spinneret orifice is extruded, the drafting rate that goes out the first coagulating bath is 6 with the ratio of the speed that spinneret orifice is extruded.Described spinning temperature is 120 ℃, described spinneret orifice draw ratio is 1.5, described the first coagulation bath composition is 35wt% solvent and excess water, temperature-5 ℃, and the speed that spinning solution goes out spinneret orifice is 10m/min, and the air gap length of described spinning solution from the spinneret orifice to the coagulating bath is 30mm.
Embodiment 7
With weight average molecular weight be 220000, structural formula (2) mixes according to 30: 70 mass ratio with solvent 1-allyl-3-methylimidazole bromine salt with the aromatic polysulfonamide that unit (molar ratio is 3: 1) in the structural formula (4) forms, at 65 ℃ of lower swelling 1h that mix of temperature, under 130 ℃, mediate dissolving 55h, obtain the spinning solution of transparent stable homogeneous.Described spinning solution is 600Pas in the apparent viscosity of 90 ℃ of lower solution of temperature.
Spinning solution enters the first coagulating bath after spinneret orifice is extruded, the drafting rate that goes out the first coagulating bath is 7.5 with the ratio of the speed that spinneret orifice is extruded.Described spinning temperature is 130 ℃, described spinneret orifice draw ratio is 1.5, described the first coagulation bath composition is 10 ℃ of 30wt% solvent and excess water, temperature, and the speed that spinning solution goes out spinneret orifice is 8m/min, and the air gap length of described spinning solution from the spinneret orifice to the coagulating bath is 30mm.
Embodiment 8
With weight average molecular weight be 180000, structural formula (1) mixes according to 35: 65 mass ratio with solvent 1-butyl-3-methylimidazole bromine salt with the aromatic polysulfonamide that unit (molar ratio is 3: 1) in the structural formula (3) forms, under temperature 70 C, mix swelling 1h, under 160 ℃, mediate dissolving 36h, obtain the spinning solution of transparent stable homogeneous.Described spinning solution is 800Pas in the apparent viscosity of 90 ℃ of lower solution of temperature.
Spinning solution enters the first coagulating bath after spinneret orifice is extruded, the drafting rate that goes out the first coagulating bath is 7 with the ratio of the speed that spinneret orifice is extruded.Described spinning temperature is 160 ℃, described spinneret orifice draw ratio is 1.5, described the first coagulation bath composition is 20 ℃ of 40wt% solvent and excess water, temperature, and the speed that spinning solution goes out spinneret orifice is 6m/min, and the air gap length of described spinning solution from the spinneret orifice to the coagulating bath is 50mm.
Claims (8)
1. aromatic polysulfonamide spinning solution with high power jet stretch ratio, it is characterized in that: the mass fraction of aromatic polysulfonamide is 5～35% in the described spinning solution, is 20～1000Pas in the apparent viscosity of 90 ℃ of lower solution of temperature; The jet stretch ratio of described spinning solution is 2～10, and namely spinning solution enters the first coagulating bath after spinneret orifice is extruded, and going out the drafting rate of the first coagulating bath and speed ratio that spinneret orifice is extruded is 2～10.
2. a kind of aromatic polysulfonamide spinning solution with high power jet stretch ratio according to claim 1, it is characterized in that, the solvent of described spinning solution viscosity at normal temperatures is greater than 0.01Pas, a kind of in 1-butyl-3-methylimidazole villaumite, 1-butyl-3-methylimidazole bromine salt, 1-allyl-3-methylimidazole bromine salt, 1-ethyl-3 methylimidazole acetate, 1-ethyl-3 methylimidazole formates or the 1-ethyl-3 methylimidazole methyl phosphite salt.
3. a kind of aromatic polysulfonamide spinning solution with high power jet stretch ratio according to claim 1, it is characterized in that described aromatic polysulfonamide is the homopolymers that is comprised of a kind of construction unit in structural formula (1)～(4) or by any two kinds of random copolymers that construction unit forms in structural formula (1)～(4);
Structural formula (1)
Structural formula (2)
Structural formula (3)
Structural formula (4)
The weight average molecular weight of described aromatic polysulfonamide is 10000～1000000.
4. a kind of aromatic polysulfonamide spinning solution with high power jet stretch ratio according to claim 3 is characterized in that, two kinds of construction unit molar ratios of the random copolymerization aromatic polysulfonamide that described any two kinds of construction units form are 1: 9～9: 1.
5. a kind of preparation method with aromatic polysulfonamide spinning solution of high power jet stretch ratio as claimed in claim 1, it is characterized in that: aromatic polysulfonamide is mixed with the mass ratio of solvent according to 5: 95～35: 65, at 20～75 ℃ of lower swelling 0.5～1h that mix of temperature, mediate the spinning solution that dissolving obtains transparent stable homogeneous at 70～160 ℃, described spinning solution is 20～1000Pas in the apparent viscosity of 90 ℃ of lower solution of temperature.
6. a kind of preparation method with aromatic polysulfonamide spinning solution of high power jet stretch ratio according to claim 5, it is characterized in that, the solvent of described spinning solution viscosity at normal temperatures is greater than 0.01Pas, a kind of in 1-butyl-3-methylimidazole villaumite, 1-butyl-3-methylimidazole bromine salt, 1-allyl-3-methylimidazole bromine salt, 1-ethyl-3 methylimidazole acetate, 1-ethyl-3 methylimidazole formates or the 1-ethyl-3 methylimidazole methyl phosphite salt.
7. a kind of preparation method with aromatic polysulfonamide spinning solution of high power jet stretch ratio according to claim 5, it is characterized in that described aromatic polysulfonamide is the homopolymers that is comprised of a kind of construction unit in structural formula (1)～(4) or by any two kinds of random copolymers that construction unit forms in structural formula (1)～(4);
Structural formula (1)
Structural formula (2)
Structural formula (3)
Structural formula (4)
The weight average molecular weight of described aromatic polysulfonamide is 10000～1000000.
8. a kind of preparation method with aromatic polysulfonamide spinning solution of high power jet stretch ratio according to claim 7, it is characterized in that two kinds of construction unit molar ratios of the random copolymerization aromatic polysulfonamide of the random copolymer that described any two kinds of construction units form are 1: 9～9: 1.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101235552A (en) * | 2008-02-29 | 2008-08-06 | 上海大学 | Random copolymerized polysulfone amide spinning solution and its preparation method |
| WO2009026482A1 (en) * | 2007-08-22 | 2009-02-26 | E.I. Du Pont De Nemours And Company | Flame resistant spun staple yarns made from blends of fibers derived from diamino diphenyl sulfone and polyoxadiazole fibers and fabrics and garments made therefrom and methods for making same |
| CN101718002A (en) * | 2009-10-21 | 2010-06-02 | 南通信一服饰有限公司 | Method for preparing ultrafine polysulfonainide fiber |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009026482A1 (en) * | 2007-08-22 | 2009-02-26 | E.I. Du Pont De Nemours And Company | Flame resistant spun staple yarns made from blends of fibers derived from diamino diphenyl sulfone and polyoxadiazole fibers and fabrics and garments made therefrom and methods for making same |
| CN101235552A (en) * | 2008-02-29 | 2008-08-06 | 上海大学 | Random copolymerized polysulfone amide spinning solution and its preparation method |
| CN101718002A (en) * | 2009-10-21 | 2010-06-02 | 南通信一服饰有限公司 | Method for preparing ultrafine polysulfonainide fiber |
Non-Patent Citations (2)
| Title |
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| 吴万涛.聚芳砜酰胺纺丝工艺与纤维结构性能研究.《东华大学硕士论文》.2010,第13、28、39、50页. |
| 聚芳砜酰胺纺丝工艺与纤维结构性能研究;吴万涛;《东华大学硕士论文》;20100101;第13、28、39、50页 * |
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