CN103526306A - Ultrasonic-assisted wet spinning device and method - Google Patents
Ultrasonic-assisted wet spinning device and method Download PDFInfo
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- CN103526306A CN103526306A CN201310467533.6A CN201310467533A CN103526306A CN 103526306 A CN103526306 A CN 103526306A CN 201310467533 A CN201310467533 A CN 201310467533A CN 103526306 A CN103526306 A CN 103526306A
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Abstract
The invention relates to an ultrasonic-assisted wet spinning device and method. According to the device, an ultrasonic auxiliary system is additionally arranged on a spinning nozzle for conventional wet spinning, and the system comprises an ultrasonic generating device, an ultrasonic transducer and an ultrasonic working head. In the process of wet spinning in a polymer solution, ultrasonic with certain power can be exerted when filaments undergo extrusion forming through the ultrasonic-assisted wet spinning device, the purpose that fibers are thinned through stretching under the action of jet flows can be achieved, and meanwhile the ultrasonic function improves flowability and spinnability of the polymer solution and accelerates material exchanges between the polymer solution and a coagulating bath solution and the process of coagulating forming of the filaments. The ultrasonic-assisted wet spinning device is easy to operate and suitable for multiple polymer systems and can effectively adjust a fiber diameter by adjusting the concentration of the polymer solution, the ultrasonic power and other parameters, and the ultrasonic-assisted wet spinning method is a novel method for effectively improving the fiber diameter.
Description
Technical field
The present invention relates to a kind of polymer wet spinning device and method, particularly a kind of ultrasonic wave auxiliary wet spinning device and method.
Background technology
Wet spinning is by certain density polymer spun silk stock solution, through filtering after deaeration, under certain pressure effect, from the aperture of spinning head, be thread shape and spray in coagulating tank, in coagulating bath, be frozen into solid-state fiber, then drawn, washing, the post processing such as dry obtain fiber.In wet spinning process, when solidifying, apply certain outfield and also must produce certain impact to the structure of fiber and performance.
Along with the change of people life style, clothes are to lightening, comfortableization, leisureization, functionalization, superior future development.Prodding and itching feeling and the sense of discomfort of textiles dress are mainly partially thick by fabric integer, and fineness is discrete causes greatly.Therefore, to the refinement of fiber, be an important technology of textile product exploitation.Fiber is carried out to refinement and reach micron order or nanoscale, can make it there is larger specific area, flexibility, compliance, slickness, stress is eliminated fast, low flexing resistance, good selvedge, and between other materials, have the good features such as interpenetrating property.The method of traditional refinement fiber is mainly divided into Physical and chemical method.Chemical method is to adopt aqueous slkali to process fiber, destroys and dissolve the scale of fiber surface, and infiltrated fiber inside disintegrates its hydrolysis gel to obtain refinement object, but chemical method length consuming time.Physical is by drawing of fiber, to reach the object of refinement, and the method is convenient and swift, but usually stretches and make fibre fineness inhomogeneous.Ultrasonic wave is that a kind of frequency is 10
4~ 10
7the elastic mechanical vibration wave of Hz.More existing research [Qian Yousan. the correlation of bamboo hemp fibre process for refining and length thereof and fineness [J]. Shanghai silk, 2004(4)] show, ultrasonic wave is processed the fiber after moulding, make the fracture propagation of fiber surface, cause fibrous refinement separated, but it is very micro-that this ultrasonic wave is processed its refining effect of fiber of moulding, fineness only becomes 18.00tex from 18.05tex.But there is not research to apply the ultrasonic impact on fibre fineness and performance in the spinning stage.
Therefore the present invention applies ultrasonic wave by polymer solution in the coagulation forming stage of wet spinning, the ultrasonic wave of certain power can discharge powerful injection stream, strand is stretched reach the object of refinement, powerful injection stream can be accelerated the effect of mass transmitting of material simultaneously.Polymer melt is applied to ultrasonic wave to be found, ultrasonic wave can obviously improve its mobility, to polymer solution effect better [Cao Yurong, Li Huilin. the impact [J] of ultrasound wave irradiation on polypropylene processing and structural behaviour. polymer material science and engineering .2001,17(3): 146-150].Therefore in wet spinning process, apply the spinnability that ultrasonic wave not only contributes to improve polymer solution, reduce spinning pressure, and under hyperacoustic effect, the mass exchange speed between polymer, solvent and poor solvent is accelerated, the coagulation forming time shorten of fiber.Therefore, when wet spinning, apply a kind of method that a ultrasound field will be effective change fibre fineness.
It is example that polysulfonamides (PSA) is take in the present invention, the organic high temperature-resistant new material that have independent intellectual property right of PSAShi China through developing for many years, there is good heat resistance and antioxygenic property, make polysulfonamides fibre there is excellent high temperature resistant, fire-retardant, electric insulation, radioresistance, chemical stability and dyeability, special uniform and the protective clothings such as suit, fire-entry suit have been applied to, fire blanket, high temperature filtration material, the fields such as encapsulant.The polysulfonamides fibre of processability excellence, to replace the high-temperature fibre (as aramid fiber 1313, Fanglun l414) of import, meet domestic dual-use need, not only there is good economic benefit, and for external monopolization, developing our high-tech industry has far-reaching strategic importance.
Summary of the invention
The defect existing for prior art, the object of the invention is to additional ultrasonic wave accessory system on a kind of existing wet spinning device, provide a kind of ultrasonic wave auxiliary wet spinning device, and utilize this device to prepare polysulfonamides fibre by wet spinning, make fiber obtain the method for refinement.
For achieving the above object, the present invention adopts following technical scheme:
The wet spinning device that ultrasonic wave is auxiliary, it comprises wet spinning system and ultrasonic wave accessory system, described wet spinning system comprises material still, filter, measuring pump, spinning head, coagulating bath; Described material still connects filter, measuring pump, spinning head successively by valve; Described ultrasonic wave accessory system comprises supersonic generator, ultrasonic transducer, ultrasonic wave working head; Described supersonic generator connects ultrasonic transducer, ultrasonic wave working head successively, and described ultrasonic wave working head is fixed on spinning head top; Spinning solution in material still is when spinning head is extruded into strand to coagulating bath, and ultrasonic wave accessory system is sent ul-trasonic irradiation in the strand of ejection, as-spun fibre is stretched and play refining effect.
The wet spinning process that ultrasonic wave is auxiliary, concrete steps are as follows:
A: the spinning solution of preparation certain mass mark;
B: ultrasonic frequency and the power of setting ultrasonic wave accessory system;
C: pour into after spinning solution deaeration in polymer material still, be extruded into strand from spinning head under certain pressure effect, coagulation forming in coagulating bath;
D: the fiber wash after moulding, oven dry, finally obtain the as-spun fibre of refinement.
The ultrasonic wave that above-mentioned ultrasonic wave accessory system is sent is continuous ultrasonic or pulse ultrasonic wave.
The ultrasonic frequency that above-mentioned ultrasonic wave accessory system is sent is 20 ~ 40kHz, and power is 20W ~ 150W.
Above-mentioned spinning solution is mass fraction 15 ~ 25% polysulfonamides/DMAc solution.
In above-mentioned coagulating bath, solution is that volume fraction is 0 ~ 60% the DMAc aqueous solution.
The diameter of above-mentioned spinning head is 0.6 ~ 1.0mm.
The pressure that spinning head in above-mentioned steps c is extruded into strand is: 0.4-0.6MPa.
The present invention can be used for polymer wet spinning, and the detailed process of spinning is as follows: polymer spun silk stock solution, under certain pressure effect, is extruded into strand from spinning head, and strand coagulation forming in coagulating bath is as-spun fibre.When introducing ultrasound field effect strand, the powerful injection stream effect of the ultrasonic wave strand that stretched, make strand refinement and make final as-spun fibre also obtain refinement, ul-trasonic irradiation has been accelerated the mobility of polymer solution, improved the spinnability of solution, accelerate the mass exchange between polymer solution and coagulating bath solution simultaneously, made strand rapid curing molding in coagulating bath, accelerated spinning speed.
Compared with prior art, the present invention has following outstanding substantive distinguishing features and significant advantage:
The present invention has increased a ultrasonic wave accessory system on traditional wet spinning device, and hyperacoustic mode of operation and power are adjustable, make polymer solution be subject to ul-trasonic irradiation in spinning moulding process, thereby improved the mobility of polymer solution, improved spinnability, and fiber has been stretched under the effect of ultrasonic wave injection stream and reach refining effect.
accompanying drawing explanation:
The schematic diagram of the wet spinning device that Fig. 1 ultrasonic wave of the present invention is auxiliary.
The auxiliary petrographic microscope photo of preparing polysulfonamides fibre of ultrasonic wave of Fig. 2 embodiment of the present invention one to six preparation.
The specific embodiment
The wet spinning of take is below prepared polysulfonamides fibre and is described the present invention as example.
As shown in Figure 1, the wet spinning device that a kind of ultrasonic wave is auxiliary, it comprises wet spinning system and ultrasonic wave accessory system, described wet spinning system comprises material still 1, filter 2, measuring pump 3, spinning head 4, coagulating bath 5; Described material still 1 connects filter 2, measuring pump 3, spinning head 4 successively by valve; Described ultrasonic wave accessory system comprises supersonic generator 6, ultrasonic transducer 7, ultrasonic wave working head 8; Described supersonic generator 6 connects ultrasonic transducer 7, ultrasonic wave working head 8 successively, and described ultrasonic wave working head 8 is fixed on spinning head 4 tops; Spinning solution in material still 1 is when spinning head 4 is extruded into strand to coagulating bath 5, and ultrasonic wave accessory system is sent ul-trasonic irradiation in the strand of ejection, as-spun fibre 9 is stretched and play refining effect.
embodiment mono-:certain polysulfonamides is dissolved into solvent N, in N-dimethylacetylamide (DMAc), preparation mass fraction is 25% polysulfonamides spinning solution, after vacuum defoamation, pour in polymer material still 1, under ultrasonic wave booster action, stoste is not extruded into strand at 0.4MPa pressure-acting from spinning head 4, and strand is at the interior coagulation forming of coagulating bath 5, the DMAc/ aqueous solution that coagulating bath 5 is 50% for volume fraction, as-spun fibre 9 washings and oven dry.Through measuring the diameter of PSA as-spun fibre, be 175.5 μ m.
embodiment bis-:certain polysulfonamides is dissolved in solvent DMA (DMAc), and preparation mass fraction is 25% polysulfonamides spinning solution, after vacuum defoamation, pours in polymer material still 1.Utilize the auxiliary wet spinning device of ultrasonic wave, spinning solution is extruded into strand at 0.4MPa pressure-acting from spinning head 4, strand is at the interior coagulation forming of coagulating bath 5, the DMAc/ aqueous solution that coagulating bath 5 is 50% for volume fraction, hyperacoustic frequency is 20kHz, power is 20W, and pattern is continuous ultrasonic.Through measuring the diameter of PSA as-spun fibre, be 118.6 μ m.
embodiment tri-:certain polysulfonamides is dissolved in solvent DMA (DMAc), and preparation mass fraction is 25% polysulfonamides spinning solution, after vacuum defoamation, pours in polymer material still 1.Utilize the auxiliary wet spinning device of ultrasonic wave, spinning solution is extruded into strand at 0.5MPa pressure-acting from spinning head 4, strand is at the interior coagulation forming of coagulating bath 5, the DMAc/ aqueous solution that coagulating bath 5 is 50% for volume fraction, hyperacoustic frequency is 20kHz, power is 50W, and pattern is continuous ultrasonic.Through measuring the diameter of PSA as-spun fibre, be 92.2 μ m.
embodiment tetra-:certain polysulfonamides is dissolved in solvent DMA (DMAc), and preparation mass fraction is 25% polysulfonamides spinning solution, after vacuum defoamation, pours in polymer material still 1.Utilize the auxiliary wet spinning device of ultrasonic wave, spinning solution is extruded into strand at 0.5MPa pressure-acting from spinning head 4, strand is at the interior coagulation forming of coagulating bath 5, the DMAc/ aqueous solution that coagulating bath 5 is 50% for volume fraction, hyperacoustic frequency is 20kHz, power is 80W, and pattern is continuous ultrasonic.Through measuring the diameter of PSA as-spun fibre, be 42.2 μ m.
embodiment five:certain polysulfonamides is dissolved in solvent DMA (DMAc), and preparation mass fraction is 25% polysulfonamides spinning solution, after vacuum defoamation, pours in polymer material still 1.Utilize the auxiliary wet spinning device of ultrasonic wave, spinning solution is extruded into strand at 0.6MPa pressure-acting from spinning head 4, strand is at the interior coagulation forming of coagulating bath 5, the DMAc/ aqueous solution that coagulating bath 5 is 50% for volume fraction, hyperacoustic frequency is 20kHz, power is 100W, and pattern is continuous ultrasonic.Through measuring the diameter of PSA as-spun fibre, be 40.7 μ m.
embodiment six:certain polysulfonamides is dissolved in solvent DMA (DMAc), and preparation mass fraction is 25% polysulfonamides spinning solution, after vacuum defoamation, pours in polymer barrel.Utilize the auxiliary wet spinning device of ultrasonic wave, spinning solution is extruded into strand at 0.6MPa pressure-acting from spinning head 4, strand is at the interior coagulation forming of coagulating bath 5, the DMAc/ aqueous solution that coagulating bath 5 is 50% for volume fraction, hyperacoustic frequency is 20kHz, power is 120W, and pattern is continuous ultrasonic.Through measuring the diameter of PSA as-spun fibre, be 49.0 μ m.
As shown in Figure 2, ultrasonic wave accessory system is sent ul-trasonic irradiation in the strand of ejection, as-spun fibre 9 is stretched and play refining effect.Hyperacoustic power is larger, and the effect of refining effect is more obvious.
Claims (8)
1. the wet spinning device that ultrasonic wave is auxiliary, it comprises wet spinning system and ultrasonic wave accessory system, it is characterized in that, described wet spinning system comprises material still (1), filter (2), measuring pump (3), spinning head (4), coagulating bath (5); Described material still (1) connects filter (2), measuring pump (3), spinning head (4) successively by valve; Described ultrasonic wave accessory system comprises supersonic generator (6), ultrasonic transducer (7), ultrasonic wave working head (8); Described supersonic generator (6) connects ultrasonic transducer (7), ultrasonic wave working head (8) successively, and described ultrasonic wave working head (8) is fixed on spinning head (4) top; Spinning solution in material still (1) is when spinning head (4) is extruded into strand to coagulating bath (5), and ultrasonic wave accessory system is sent ul-trasonic irradiation in the strand of ejection, makes as-spun fibre (9) be stretched and play refining effect.
2. the auxiliary wet spinning process of ultrasonic wave, is characterized in that, concrete steps are as follows:
A: the spinning solution of preparation certain mass mark;
B: ultrasonic frequency and the power of setting ultrasonic wave accessory system;
C: pour into after spinning solution deaeration in polymer material still (1), be extruded into strand from spinning head (4) under certain pressure effect, coagulation forming in coagulating bath (5);
D: the fiber wash after moulding, oven dry, finally obtain the as-spun fibre (9) of refinement.
3. the auxiliary wet spinning process of ultrasonic wave according to claim 2, is characterized in that, the ultrasonic wave that described ultrasonic wave accessory system is sent is continuous ultrasonic or pulse ultrasonic wave.
4. the auxiliary wet spinning process of ultrasonic wave according to claim 2, is characterized in that, the ultrasonic frequency that described ultrasonic wave accessory system is sent is 20 ~ 40kHz, and power is 20W ~ 150W.
5. the auxiliary wet spinning process of ultrasonic wave according to claim 2, is characterized in that, described spinning solution is mass fraction 15 ~ 25% polysulfonamides/DMAc solution.
6. the auxiliary wet spinning process of ultrasonic wave according to claim 2, is characterized in that, in described coagulating bath (5), solution is that volume fraction is 0 ~ 60% the DMAc aqueous solution.
7. the auxiliary wet spinning process of ultrasonic wave according to claim 2, is characterized in that, the diameter of described spinning head (4) is 0.6 ~ 1.0mm.
8. the auxiliary wet spinning process of ultrasonic wave according to claim 2, is characterized in that, the pressure that the spinning head in described step c (4) is extruded into strand is: 0.4-0.6MPa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105780153A (en) * | 2016-05-09 | 2016-07-20 | 福建师范大学泉港石化研究院 | Ultrasonic assistant electrostatic spinning device |
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| CN101187078A (en) * | 2007-12-13 | 2008-05-28 | 东华大学 | Preparation method of carbon nanometer tube/ polyimide composite fiber |
| DE102009009107A1 (en) * | 2009-02-16 | 2010-08-19 | Fleissner Gmbh | Filaments stretching method, involves guiding filaments in form of cables around powered godets of stretching units, and pressurizing cables to be stretched with ultrasonic radiation, and coupling ultrasonic field into cables |
| CN102698611A (en) * | 2012-06-27 | 2012-10-03 | 上海大学 | Method for preparing polysulfone amide hollow fiber separation membrane by wet spinning |
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2013
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| CN1093761A (en) * | 1992-07-23 | 1994-10-19 | 纳幕尔杜邦公司 | The quenching of long filament and solidifying in ultrasonic wave |
| CN101187078A (en) * | 2007-12-13 | 2008-05-28 | 东华大学 | Preparation method of carbon nanometer tube/ polyimide composite fiber |
| DE102009009107A1 (en) * | 2009-02-16 | 2010-08-19 | Fleissner Gmbh | Filaments stretching method, involves guiding filaments in form of cables around powered godets of stretching units, and pressurizing cables to be stretched with ultrasonic radiation, and coupling ultrasonic field into cables |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105780153A (en) * | 2016-05-09 | 2016-07-20 | 福建师范大学泉港石化研究院 | Ultrasonic assistant electrostatic spinning device |
| CN105780153B (en) * | 2016-05-09 | 2017-12-22 | 福建师范大学泉港石化研究院 | A kind of ultrasonic wave added electrostatic spinning apparatus |
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Application publication date: 20140122 |