CN103409847A - Preparation method of polyphenylene sulfide superfine fiber - Google Patents
Preparation method of polyphenylene sulfide superfine fiber Download PDFInfo
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- CN103409847A CN103409847A CN201310390969XA CN201310390969A CN103409847A CN 103409847 A CN103409847 A CN 103409847A CN 201310390969X A CN201310390969X A CN 201310390969XA CN 201310390969 A CN201310390969 A CN 201310390969A CN 103409847 A CN103409847 A CN 103409847A
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Abstract
The invention relates to a preparation method of polyphenylene sulfide superfine fiber. The preparation method comprises the following steps: uniformly mixing fiber-grade polyphenylene sulfide with polyamide; melting, blending and spinning under the technological condition of not only controlling PPS (Polyphenylene Sulfide) to be molten for processing, but also enabling PA (Polyamide) not to decompose, placing the obtained polyphenylene sulfide/polyamide blended sea-island fiber in an organic solvent; and enabling the polyamine to dissolve in the corresponding organic solvent under the normal temperature condition to obtain the polyphenylene sulfide superfine fiber with a diameter range of 20nm-400nm. The preparation method of the polyphenylene sulfide superfine fiber disclosed by the invention is simple and efficient, free of a third component compatilizer, low in peel-off temperature, low in bath ratio, high in peel-off efficiency, small in energy consumption and capable of carrying out peeling completely. Moreover, the superfine fiber has the characteristics including strong adsorption capacity, softness, high temperature resistance, flame resistance, solvent resistance, high strength and the like.
Description
Technical field
The present invention relates to superfine fibre, particularly adopt fiber-grade polyphenyl thioether and polyamide blended melt spinning to prepare the method for polyphenylene sulfide superfine fibre, and the polyphenylene sulfide superfine fibre obtained by this preparation method.
Background technology
Superfine fibre reaches domestic not definite generally acknowledged definition in the world, but the definition that most people accept is the belong to superfine fibre of single fiber density at 0.1-1.0dtex.The reduction of fiber linear density has given fiber a lot of good performances, such as yarn strength is high, flexibility is good, drapability is good, adsorptivity is strong, dirt-removing power is strong, filterability is good, capillary effect is good, have simultaneously the characteristics that the multinomial premium properties such as waterproof and breathable are integrated.Therefore, space material, industrial production, home wear with in all be widely used.
The preparation method of superfine fibre has a variety of, comprise direct spinning, composite spinning method, blend island method, hubbing, template synthetic method, interfacial polymerization, phase separation method, bioanalysis and flash-spinning method etc., wherein industrialized technology has direct spinning, composite spinning method and co-blended spinning method.Wherein, the fibre fineness simple, that produce of the technical equipment due to co-blended spinning is little, controllability is strong, cost is low, efficiency is high, has obtained degree of recognition widely.
Polyphenylene sulfide is a kind of macromolecular compound with aromatic rings, has the excellent properties such as high-crystallinity, outstanding heat endurance, radiation resistance, wear-resisting, resist chemical, high strength.Therefore in a plurality of fields such as the filtration of heat chemistry product, electrically insulating material making, radiation proof space material, special dimension protective clothing, insulation material, reinforcing materials, have broad application prospects.If the diameter of polyphenylene sulfide fibre is reduced to 1 μ m even below 500nm, can improves so porosity between the specific area, fiber of fiber, and then improve filter effect.Simultaneously, the fine of polyphenylene sulfide fibre also will promote it in many-sided application, improve in clothes comfort level, insulation material greatly effect of performance in fields such as improving the material softness degree such as in composite, strengthening in interfacial tension, radiation proof space material.In the present invention, utilize blend island spin processes to prepare the superfine fibre of polyphenylene sulfide, make the fineness of polyphenylene sulfide fibre reach 20-400nm, reduce fibre diameter, increase pulp freeness, promote the development for preparing the high-performance superfine fiber.
In order to reduce costs, need to improve the ratio of polyphenylene sulfide in blend.But polyphenylene sulfide content increases, especially surpass 50wt%, be difficult for forming decentralized photo.Even the formation decentralized photo, the shared ratio of polyphenylene sulfide is higher, and decentralized photo polyphenylene sulfide island phase diameter also can increase, and affects the final performance of product.
In existing patent, the co-blended spinning of open polyphenylene sulfide and polyamide, disclose a kind of method for preparing large diameter fire resistant polyphenylene sulfide blended fibre as CN101161329A, and CN1948564A discloses a kind of method for preparing polyphenyl thioether complex fiber.This case inventor, by research, has chosen polyphenylene sulfide, polyamide blended system, by selecting melt viscosity ratio and the processing conditions of suitable blend components, develops the polyphenylene sulfide superfine fibre of high ratio of components.Preparation method's production efficiency of the present invention is high, and cost is low, is easy to suitability for industrialized production.
Summary of the invention
The purpose of this invention is to provide a kind of method that adopts polyphenylene sulfide and polyamide blended melt spinning to be prepared the polyphenylene sulfide superfine fibre.
Another object of the present invention is to provide the polyphenylene sulfide superfine fibre that adopts polyphenylene sulfide and polyamide blended melt spinning to prepare.
The preparation method of polyphenylene sulfide superfine fibre of the present invention comprises the following steps:
(1) fiber-grade polyphenyl thioether of 30-70 parts by mass (being preferably the 50-60 parts by mass) is mixed with the polyamide of 70-30 parts by mass (being preferably the 50-40 parts by mass), then join in extruder type spinning machine and carry out blended melting extruding spinning, polyphenylene sulfide/polyamide blended the fiber of the coming into being HEAT SETTING that stretches under 120 ℃ of conditions, draw ratio 2-3 doubly, the drawn HEAT SETTING prepares polyphenylene sulfide/polyamide blended islands-in-sea type fibre:
(2) polyphenylene sulfide step (1) obtained/polyamide blended islands-in-sea type fibre is placed in organic solvent (formic acid), and described polyamide is dissolved in described organic solvent to remove the polyamide in blended fiber, obtains the polyphenylene sulfide superfine fibre.
Described fiber-grade polyphenyl thioether melt index is 100-120g/10min.
The relative viscosity of described polyamide is 2.5-3.0.
Described polyamide is polycaprolactam or polyhexamethylene adipamide, is preferably polycaprolactam.
The temperature of the blended melting described in step (1) extruding spinning is 275-295 ℃.
Organic solvent described in step (2) is the organic solvent of the described polyamide of solubilized, is preferably formic acid.While dissolving described polyamide, need temperature constant state, typical temperature is 15-30 ℃, and the time of dissolving is 1-3 hour.
The polyphenylene sulfide superfine fibre component obtained by preparation method of the present invention is 100% polyphenylene sulfide; The single fiber diameter of polyphenylene sulfide superfine fibre is 20-400nm, and preferably the single fiber diameter of described polyphenylene sulfide superfine fibre is 30-300nm.
In the methods of the invention, by regulation and control polyphenylene sulfide and polyamide blended mass fraction ratio, with control, prepare polyphenylene sulfide under different proportion/polyamide blended fiber, to obtain polyphenylene sulfide superfine fibre at high proportion.In the present invention, the preparation method of superfine fibre is simple, does not need to add the 3rd component compatibility agent, just can prepare island and be evenly distributed mutually, the thin and polyphenylene sulfide superfine fibre that is easy to peel off of diameter.Simultaneously, for the molten organic solvent removed, can realize recycling in the present invention, environmentally friendly, and can in polyphenylene sulfide superfine fibre process units, be achieved, be easy to form the production of scale.
The diameter of the polyphenylene sulfide superfine fibre of preparing according to preparation method of the present invention is 20-400nm, this superfine fibre, owing to having the excellent properties such as good feel, heat endurance, radiation hardness, wear-resisting, resist chemical, high strength, can be applicable to the aspects such as the filtration of heat chemistry product, electrically insulating material making, radiation proof space material clothes, insulation material, reinforcing material.
The accompanying drawing explanation
Fig. 1 is the superfine fibre stereoscan photograph that the embodiment of the present invention 1 prepares
Fig. 2 is the superfine fibre stereoscan photograph that the embodiment of the present invention 2 prepares
Fig. 3 is the superfine fibre stereoscan photograph that the embodiment of the present invention 3 prepares
Fig. 4 is the superfine fibre stereoscan photograph that the embodiment of the present invention 4 prepares
Fig. 5 is the superfine fibre stereoscan photograph that the embodiment of the present invention 5 prepares
The specific embodiment
The present invention is further illustrated below in conjunction with specific embodiment, but described embodiment is be used to the present invention is described, and be not limited only to the present invention.
By melt index be the fiber-grade polyphenyl thioether section of 110g/10min in vacuum drying oven with 120 ℃ of dryings 12 hours, by relative viscosity be 2.8 polyamide section in vacuum drying oven with 90 ℃ of dryings 12 hours.Both be take to polyphenylene sulfide/polyamide after the even blend of 40/60 mass fraction, put into extruder type spinning machine and carry out co-blended spinning, 285 ℃ of spinning temperatures, polyphenylene sulfide/polyamide blended fiber drawing and heat-setting under 120 ℃ of conditions of coming into being, 3 times of drafting multiples, obtain constitutionally stable polyphenylene sulfide/polyamide blended fiber, the intensity of blended fiber can reach 5.74cN/dtex.
By polyphenylene sulfide/polyamide blended fiber in formic acid solution with molten removing under 25 ℃ of conditions, molten except the time be 1-3 hour, obtain the polyphenylene sulfide superfine fibre.Fibre diameter be distributed as 25-205nm, average diameter is about 90nm.
Embodiment 2
By melt index be the fiber-grade polyphenyl thioether section of 110g/10min in vacuum drying oven with 120 ℃ of dryings 12 hours, by relative viscosity be 2.8 polyamide section in vacuum drying oven with 90 ℃ of dryings 12 hours.Both be take to polyphenylene sulfide/polyamide after 50/50 mass fraction blend evenly, put into extruder type spinning machine and carry out co-blended spinning, 285 ℃ of spinning temperatures, polyphenylene sulfide/polyamide blended fiber drawing and heat-setting under 120 ℃ of conditions of coming into being, 2 times of drafting multiples, obtain constitutionally stable polyphenylene sulfide/polyamide blended fiber, the intensity of blended fiber can reach 2.59cN/dtex.
By polyphenylene sulfide/polyamide blended fiber in formic acid solution with molten removing under 25 ℃ of conditions, molten except the time be 1-2.5 hour, obtain the polyphenylene sulfide superfine fibre.Fibre diameter be distributed as 45-277nm, average diameter is about 119nm.
Embodiment 3
By melt index be the fiber-grade polyphenyl thioether section of 110g/10min in vacuum drying oven with 120 ℃ of dryings 12 hours, by relative viscosity be 2.8 polyamide section in vacuum drying oven with 90 ℃ of dryings 12 hours.Both be take to polyphenylene sulfide/polyamide after 50/50 mass fraction blend evenly, put into extruder type spinning machine and carry out co-blended spinning, 285 ℃ of spinning temperatures, polyphenylene sulfide/polyamide blended fiber drawing and heat-setting under 120 ℃ of conditions of coming into being, 3 times of drafting multiples, obtain constitutionally stable polyphenylene sulfide/polyamide blended fiber altogether, the intensity of combined filament can reach 3.69cN/dtex.
By polyphenylene sulfide/polyamide blended fiber in formic acid solution with molten removing under 25 ℃ of conditions, molten except the time be 1-2.5 hour, obtain the polyphenylene sulfide superfine fibre.Fibre diameter be distributed as 39-304nm, average diameter is about 95nm.
Embodiment 4
By melt index be the fiber-grade polyphenyl thioether section of 110g/10min in vacuum drying oven with 120 ℃ of dryings 12 hours, by relative viscosity be 2.8 polyamide section in vacuum drying oven with 90 ℃ of dryings 12 hours.Both be take to polyphenylene sulfide/polyamide after 55/45 mass fraction blend evenly, put into extruder type spinning machine and carry out co-blended spinning, 285 ℃ of spinning temperatures, polyphenylene sulfide/polyamide blended fiber drawing and heat-setting under 120 ℃ of conditions of coming into being, 3 times of drafting multiples, obtain constitutionally stable polyphenylene sulfide/polyamide blended fiber, the intensity of blended fiber can reach 3.30cN/dtex.
By polyphenylene sulfide/polyamide blended fiber in formic acid solution with molten removing under 25 ℃ of conditions, molten except the time be 1-2 hour, obtain the polyphenylene sulfide superfine fibre.Fibre diameter be distributed as 52-268nm, average diameter is about 139nm.
Embodiment 5
By melt index be the fiber-grade polyphenyl thioether section of 110g/10min in vacuum drying oven with 120 ℃ of dryings 12 hours, by relative viscosity be 2.8 polyamide section in vacuum drying oven with 90 ℃ of dryings 12 hours.Both be take to polyphenylene sulfide/polyamide after 60/40 mass fraction blend evenly, put into extruder type spinning machine and carry out co-blended spinning, 285 ℃ of spinning temperatures, polyphenylene sulfide/polyamide blended fiber drawing and heat-setting under 120 ℃ of conditions of coming into being, 3 times of drafting multiples, obtain constitutionally stable polyphenylene sulfide/polyamide blended fiber, the intensity of blended fiber can reach 4.73cN/dtex.
By polyphenylene sulfide/polyamide blended fiber in formic acid solution with molten removing under 25 ℃ of conditions, molten except the time be 1-3 hour, obtain the polyphenylene sulfide superfine fibre.Fibre diameter be distributed as 62-407nm, average diameter is about 131nm.
Claims (10)
1. the preparation method of a polyphenylene sulfide superfine fibre, is characterized in that, described preparation method comprises the following steps:
(1) fiber-grade polyphenyl thioether of 30-70 parts by mass is mixed with the polyamide section of 70-30 parts by mass, then join in extruder type spinning machine and carry out melt blending extruding spinning, the drawn HEAT SETTING, make polyphenylene sulfide/polyamide blended islands-in-sea type fibre;
(2) polyphenylene sulfide step (1) obtained/polyamide blended islands-in-sea type fibre is placed in organic solvent, and described polyamide is dissolved in corresponding organic solvent to remove the polyamide in blended fiber, obtains the polyphenylene sulfide superfine fibre.
2. preparation method according to claim 1, is characterized in that, the melt index of described fiber-grade polyphenyl thioether is 100-120g/10min.
3. preparation method according to claim 1, is characterized in that, the solution temperature while dissolving polyamide in described step (2) is 15-30 ℃, and the time of dissolving is 1-3 hour.
4. preparation method according to claim 1, is characterized in that, described polyamide is polycaprolactam or polyhexamethylene adipamide.
5. preparation method according to claim 1, is characterized in that, the relative viscosity of described polyamide is 2.5-3.0.
6. preparation method according to claim 1, is characterized in that, described organic solvent is formic acid.
7. preparation method according to claim 1, is characterized in that, the temperature of the blended melting described in step (1) extruding spinning is 275-295 ℃.
8. preparation method according to claim 1, is characterized in that, the HEAT SETTING that stretches under 120 ℃ of conditions, and draw ratio is 2-3 times.
9. preparation method according to claim 1, is characterized in that, the fiber-grade polyphenyl thioether consumption is the 50-60 parts by mass, and the polyamide consumption is the 50-40 parts by mass.
10. the polyphenylene sulfide superfine fibre obtained by the described preparation method of claim 1-9 any one, is characterized in that, the filamentary diameter of described polyphenylene sulfide superfine fibre is 20-400nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103774277A (en) * | 2014-01-15 | 2014-05-07 | 北京服装学院 | Polyphenylene sulfide superfine fiber and preparation method thereof |
| CN104894752A (en) * | 2015-05-08 | 2015-09-09 | 江苏瑞泰科技有限公司 | Method for producing superfine denier abnormity polyphenylene sulfide non-woven fabrics |
| CN113151930A (en) * | 2021-05-20 | 2021-07-23 | 东华大学 | Sea-island polyphenylene sulfide superfine fiber and preparation method thereof |
Citations (5)
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| JPH04333618A (en) * | 1991-04-30 | 1992-11-20 | Toray Ind Inc | Polyphenylene sulfide conjugate fiber |
| CN1310251A (en) * | 2001-01-05 | 2001-08-29 | 南亚塑胶工业股份有限公司 | Superfine fiber and its making process |
| CN101302665A (en) * | 2008-05-21 | 2008-11-12 | 四川大学 | Polyarylene sulfide superfine fibre and preparation thereof |
| CN102071495A (en) * | 2010-07-28 | 2011-05-25 | 烟台万华超纤股份有限公司 | Figured sea-island super-fine fiber, and preparation method thereof and synthetic leather preparing process method using same |
| CN102345188A (en) * | 2010-07-23 | 2012-02-08 | 东丽纤维研究所（中国）有限公司 | Polymer alloy fiber and polyphenylene sulfide (PPS) ultrafine fiber |
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2013
- 2013-09-01 CN CN201310390969.XA patent/CN103409847B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04333618A (en) * | 1991-04-30 | 1992-11-20 | Toray Ind Inc | Polyphenylene sulfide conjugate fiber |
| CN1310251A (en) * | 2001-01-05 | 2001-08-29 | 南亚塑胶工业股份有限公司 | Superfine fiber and its making process |
| CN101302665A (en) * | 2008-05-21 | 2008-11-12 | 四川大学 | Polyarylene sulfide superfine fibre and preparation thereof |
| CN102345188A (en) * | 2010-07-23 | 2012-02-08 | 东丽纤维研究所（中国）有限公司 | Polymer alloy fiber and polyphenylene sulfide (PPS) ultrafine fiber |
| CN102071495A (en) * | 2010-07-28 | 2011-05-25 | 烟台万华超纤股份有限公司 | Figured sea-island super-fine fiber, and preparation method thereof and synthetic leather preparing process method using same |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103774277A (en) * | 2014-01-15 | 2014-05-07 | 北京服装学院 | Polyphenylene sulfide superfine fiber and preparation method thereof |
| CN103774277B (en) * | 2014-01-15 | 2016-03-30 | 北京服装学院 | A kind of polyphenylene sulfide superfine fiber and preparation method thereof |
| CN104894752A (en) * | 2015-05-08 | 2015-09-09 | 江苏瑞泰科技有限公司 | Method for producing superfine denier abnormity polyphenylene sulfide non-woven fabrics |
| CN104894752B (en) * | 2015-05-08 | 2017-10-13 | 江苏瑞泰科技有限公司 | A kind of production method of the special-shaped polyphenylene sulfide non-woven fabrics of super fine denier |
| CN113151930A (en) * | 2021-05-20 | 2021-07-23 | 东华大学 | Sea-island polyphenylene sulfide superfine fiber and preparation method thereof |
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