CN102605446A - Annular blowing cooling solidification process method for preparing polyvinyl alcohol fibre - Google Patents
Annular blowing cooling solidification process method for preparing polyvinyl alcohol fibre Download PDFInfo
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- CN102605446A CN102605446A CN2012100787747A CN201210078774A CN102605446A CN 102605446 A CN102605446 A CN 102605446A CN 2012100787747 A CN2012100787747 A CN 2012100787747A CN 201210078774 A CN201210078774 A CN 201210078774A CN 102605446 A CN102605446 A CN 102605446A
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Abstract
The invention relates to an annular blowing cooling solidification process method for preparing polyvinyl alcohol fiber. The method has the characteristics that the annular blowing cooling technique to cool a polyvinyl alcohol melt extruded from a spinneret plate in a melt spinning is adopted; by controlling various annular blowing process parameters, the annular blowing wind speed is 0.6 to 3.5m/s, the air temperature is 21 to 25 degrees centigrade, the humidity is 30 to 55%, the annular blowing height is 0.3 to 1.8m, therefore, the turbulence of a cold air is removed to enable the spun raw filament to be uniformly cooled, improve the stability of spinning, lower the spinning flaw and improve the uniformity of spun fiber section and further better control the water content of spun fibers to be good for realizing high stretching to manufacture the high-performance polyvinyl alcohol fiber with uniform strength and fineness and high modulus and suitable for being used as the reinforcing material in concrete.
Description
Technical field
The present invention relates to a kind of ring blowing cooled and solidified process for preparing vinal, particularly relate to a kind of ring blowing cooled and solidified process for preparing control polyvinyl alcohol moisture in the vinal.
Background technology
The vinal price is low, density is little, cohesive force is high, good dispersion, be easy to stir; Compare with other synthetic fiber; Vinal good hydrophilic property, elastic modelling quantity height; And have high-specific surface area, good with the cement concrete compatibility, be applicable to the reinforcing material in the concrete; Characteristics such as the concrete tensile property is poor to improve, performance of resisting cracking difference and ductility difference, reinforced effects is obvious.
Cooled and solidified technology is an important step in the polyvinyl alcohol spinning process, and the melt thread needs cooling to make it solidify the formation as-spun fibre before spinnerets is ejected into boundling, its objective is that the melt thread is evenly cooled off as early as possible forms stable as-spun fibre.At present, the solidified forming of vinal adopts coagulating bath more, like wet spinning and gel spinning; But the two-way mass transport process of these spinning process makes the vinal structure inhomogeneous; The cross section is kidney shape, and tangible skin-core structure is arranged, and can't bear super drawing; Can not reach the thick dawn standard of the fortifying fibre that civil engineering uses, cause dispersiveness and the reinforced effects of fiber in concrete not good.And wet spinning great majority employing polyvinyl alcohol of high degree of polymerization, additive is complicated, needs follow-up extraction process, and production cost is high, and environmental pollution is big.
The above-mentioned variety of problems that melt spinning can avoid these spinning process to occur, and shrink during the melt-spinning fiber moulding for a short time, the fibre section uniformity is high, can impose super drawing, thereby improves fibre property.Polyvinyl alcohol is a water-soluble high-molecular material, contacts with water to make fiber surface swelling stickness, the stretching of fiber is had very big influence, and then limited its apparent and serviceability, so can't adopt water-cooling process.Therefore, the cooled and solidified of polyvinyl alcohol melt spinning is the problem that remains our solution.The method that 200510057435.0 1 kinds of patents prepare high performance polyvinyl alcohel fiber has realized the cooled and solidified technology of polyvinyl alcohol melt spinning with the mode of lateral blowing; Its lateral blowing temperature: 10～80 ℃; Humidity: 65～85%, solved the cooling problem of polyvinyl alcohol as-spun fibre.But the cooling air humidity is big in the above-mentioned technology, to removing the plasticizer water poor effect in the polyvinyl alcohol melt, and excess moisture or very fewly all can influence after-drawing; This technology does not limit cold air blast velocity yet simultaneously; The cooling velocity of wind speed restriction as-spun fibre has influenced the performance of as-spun fibre, causes that fibre number is irregular, intensity is irregular, evenness fault (the CV value is bigger) etc.; In addition, this technology does not reach the purpose of control polyvinyl alcohol as-spun fibre moisture.
Summary of the invention
The objective of the invention is in order to overcome technological deficiency recited above, a kind of ring blowing cooled and solidified process for preparing vinal is provided.Both made as-spun fibre evenly cooled off the stability that guarantees spinning with this process for cooling; The moisture of controlling fiber effectively again; The as-spun fibre that obtains has littler fiber number and intensity irregularity; Make its requirement that reaches following process, can make high-performance polyethylene alcohol coarse denier fiber, can be widely used in the architectural engineering concrete field.
In order to solve technical problem recited above, the present invention takes following technical scheme:
The invention provides a kind of ring blowing cooled and solidified process for preparing vinal, the polyvinyl alcohol melt is extruded from spinnerets, boundling after the blowing cooling forms as-spun fibre; The mode of ring blowing is adopted in described blowing cooling; The blowing of described ring is annular horizontal blowing cooling, promptly cools off air and flows perpendicular to the strand traffic direction and around tow, blow to strand, and technological parameter is: wind speed 0.6～3.5m/s; 21～25 ℃ of wind-warm syndrome, humidity 30～55%; Described polyvinyl alcohol melt is meant with water to be the molten polyethylene alcohol of plasticizer; The described polyvinyl alcohol degree of polymerization is 1500～2600, and alcoholysis degree is 88～99%.
As optimized technical scheme:
Aforesaid a kind of ring blowing cooled and solidified process for preparing vinal, described ring blowing highly is 0.3～1.8m.
Aforesaid a kind of ring blowing cooled and solidified process for preparing vinal, the moisture of described polyvinyl alcohol melt is 30～60wt%.The adding of water helps the heating and melting of polyvinyl alcohol, improves spinnability, and the after-drawing to fiber simultaneously also has certain influence.
Aforesaid a kind of ring blowing cooled and solidified process for preparing vinal; Also comprise the compound that can form hydrogen bond in the described polyvinyl alcohol melt, i.e. nitrogen-containing compound, hydroxy-containing compounds, sulfur-containing compound or carboxylated compound with the hydroxyl in the polyvinyl alcohol.These materials account for polyvinyl alcohol melt gross mass 1～20wt%, generally are micromolecule or oligomer plasticizer, and they are to realize the most direct and effective method of polyvinyl alcohol melt spinning.
Aforesaid a kind of ring blowing cooled and solidified process for preparing vinal, described nitrogen-containing compound is caprolactam, polyamide or aqueous polyurethane; Hydroxy-containing compounds is that glycerine, monoethanolamine or molecular weight are 200～2000 polyethylene glycol; Sulfur-containing compound is an ethylene thiourea; Carboxylated compound is citric acid or tartaric acid.
The most frequently used nitrogen-containing compound is a caprolactam.Caprolactam and polyvinyl alcohol have complementary structure, form compound modifier with water, can destroy in polyvinyl alcohol self molecule and intermolecular hydrogen bonding; Suppress the crystallization of polyvinyl alcohol, reduce its fusing point, and through the hydrogen bond between polyvinyl alcohol and caprolactam and hydrone; Reduce free water content; Realize the superheat of water in polyvinyl alcohol, under processing temperature, do not produced bubble, realized its melt spinning.Higher boiling glycerine is the most frequently used polyalcohols plasticizer, glycerine can increase polyvinyl alcohol the segment activity, reduce crystal region, thereby reduce fusing point.But the plasticization effect of glycerine reduces along with the increase of glycerol content gradually, and plasticization effect sharply reduces when being separated.The adding of single plasticizer is difficult to realize the thermoplastic processing of polyvinyl alcohol, and it is better different plasticizer to be joined in the polyvinyl alcohol plasticization effect after compound.
Aforesaid a kind of ring blowing cooled and solidified process for preparing vinal, described wind speed is 1.5m/s, and wind-warm syndrome is 23 ℃, and humidity is 45%.Cooperatively interacting of wind speed, rheumatism and humidity guaranteed in certain cooling range, to be defined as away the heat and the moisture of strand, and strand is evenly cooled off, and the strand of avoiding the air turbulence to cause vibrates or waves.
Aforesaid a kind of ring blowing cooled and solidified process for preparing vinal, described as-spun fibre moisture is 15～40wt%.Ring blowing technology has been removed the part moisture in the spun filament, sends into drying device then and adjusts fiber moisture content once more, until the condition that reaches suitable tensile fiber.The ring blowing is a master operation of regulation and control fiber moisture content, and most moisture is taken away by air in this process.
Ring blowing is a kind of cooling curing method of the strand from spinnerets, extruded in the spinning technique process.The cooling air gets into the ring blowing device from distributing pipe; Through cowling panel change into horizontal direction from around blow to tow, through all conditions of wind speed, wind-warm syndrome and the humidity of control blowing, keep all in constant environment, being cooled from the melt of spinnerets ejection; Guarantee that fibre forming is stable, quality is even.The ring blowing belongs to the pressure heat exchange, helps the strand cooling evenly, and it is stable to be shaped, and makes strand cross section structure homogeneous, can guarantee cooling effect simultaneously, helps improving spinning quality.
Good effect of the present invention is embodied in:
(1) adopts the ring cold wind blower, do not need coagulating bath, only remove the plasticizer water of polyvinyl alcohol through unidirectional mass transfer.When adopting the ring blowing air with thread become vertical direction directly from around blow on strand; Heat transfer coefficient is higher; Cooling has evenly overcome that air nature cooling velocity is slow, efficient is low, follow-up draft process is difficult to carry out, can't reach the shortcoming of large scale industry production requirement, and the as-spun fibre fiber number that obtains, intensity improve; Yarn unevenness is lower, and the CV value is reduced to below 5%.And the ring blowing device has been eliminated the turbulent flow of cold wind basically; The temperature difference of tow blowing in cabinet, lee face reduces greatly; The cooling velocity of tow ectonexine more is tending towards homogenization, for stablizing spinning technique, reduces the spinning fault and has created condition with the uniformity of improving the as-spun fibre cross section.
(2) optimize ring blowing parameters; This polyvinyl alcohol coarse denier as-spun fibre is evenly cooled off; Make from the high polymer molten cool to room temperature of spinneret orifice ejection and form as-spun fibre, and effectively controlled the moisture of as-spun fibre, both satisfied of the requirement of as-spun fibre high-tenacity the high stretching ratio of back processing; Improve the tensile property of as-spun fibre, guaranteed the higher running rate of back processing unit (plant) again.
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 to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to 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 institute restricted portion equally.
Embodiment 1
With the polyethylene alcohol and water of the degree of polymerization 1700, alcoholysis degree 88% under stirring action in closed container swelling, wherein water accounts for 30% of both gross masses.Fully the polyvinyl alcohol after the swelling is used the double screw extruder spinning, and melt sprays from spinnerets, through ring blowing cooling; Wind speed 0.6m/s, 21 ℃ of wind-warm syndrome, humidity 30%; Ring blowing highly be 0.3m, cools off boundling afterwards, obtains moisture and be 22% polyvinyl alcohol as-spun fibre.
Embodiment 2
With the polyethylene alcohol and water of the degree of polymerization 2600, alcoholysis degree 99% under stirring action in closed container swelling, wherein water accounts for 60% of both gross masses.Fully the polyvinyl alcohol after the swelling is used the double screw extruder spinning, and melt sprays from spinnerets, through ring blowing cooling; Wind speed 3.5m/s, 25 ℃ of wind-warm syndrome, humidity 55%; Ring blowing highly be 1.8m, cools off boundling afterwards, obtains moisture and be 30% polyvinyl alcohol as-spun fibre.
Embodiment 3
With the polyethylene alcohol and water of the degree of polymerization 2000, alcoholysis degree 99% under stirring action in closed container swelling, wherein water accounts for 45% of both gross masses.Fully the polyvinyl alcohol after the swelling is used the double screw extruder spinning, and melt sprays from spinnerets, through ring blowing cooling; Wind speed 1.5m/s, 23 ℃ of wind-warm syndrome, humidity 45%; Ring blowing highly be 1.1m, cools off boundling afterwards, obtains moisture and be 16% polyvinyl alcohol as-spun fibre.
Embodiment 4
With the polyethylene alcohol and water of the degree of polymerization 2400, alcoholysis degree 99% under stirring action in closed container swelling, wherein water accounts for 24% of both gross masses.Fully the polyvinyl alcohol after the swelling is used the double screw extruder spinning, and melt sprays from spinnerets, through ring blowing cooling; Wind speed 1.7m/s, 24 ℃ of wind-warm syndrome, humidity 45%; Ring blowing highly be 1.4m, cools off boundling afterwards, obtains moisture and be 16% polyvinyl alcohol as-spun fibre.
Embodiment 5
With the polyvinyl alcohol of the degree of polymerization 1700, alcoholysis degree 99%, caprolactam and water under stirring action in closed container swelling, wherein water accounts for 40% of three's gross mass, caprolactam accounts for 5% of three's gross mass.Fully the polyvinyl alcohol after the swelling is used the double screw extruder spinning, and melt sprays from spinnerets, through ring blowing cooling; Wind speed 1.6m/s, 24 ℃ of wind-warm syndrome, humidity 40%; Ring blowing highly be 1.2m, cools off boundling afterwards, obtains moisture and be 18% polyvinyl alcohol as-spun fibre.
Embodiment 6
With the polyvinyl alcohol of the degree of polymerization 1700, alcoholysis degree 92%, polyamide and water under stirring action in closed container swelling, wherein water accounts for 30% of three's gross mass, polyamide accounts for 7% of three's gross mass.Fully the polyvinyl alcohol after the swelling is used the double screw extruder spinning, and melt sprays from spinnerets, through ring blowing cooling; Wind speed 1.5m/s, 23 ℃ of wind-warm syndrome, humidity 45%; Ring blowing highly be 1m, cools off boundling afterwards, obtains moisture and be 17% polyvinyl alcohol as-spun fibre.
Embodiment 7
With the polyvinyl alcohol of the degree of polymerization 2400, alcoholysis degree 99%, aqueous polyurethane and water under stirring action in closed container swelling, wherein water accounts for 50% of three's gross mass, aqueous polyurethane accounts for 8% of three's gross mass.Fully the polyvinyl alcohol after the swelling is used the double screw extruder spinning, and melt sprays from spinnerets, through ring blowing cooling; Wind speed 1.3m/s, 23 ℃ of wind-warm syndrome, humidity 52%; Ring blowing highly be 0.8m, cools off boundling afterwards, obtains moisture and be 23% polyvinyl alcohol as-spun fibre.
Embodiment 8
With the polyvinyl alcohol of the degree of polymerization 1700, alcoholysis degree 99%, G & W under stirring action in closed container swelling, wherein water accounts for 45% of three's gross mass, glycerine accounts for 15% of three's gross mass.Fully the polyvinyl alcohol after the swelling is used the double screw extruder spinning, and melt sprays from spinnerets, through ring blowing cooling; Wind speed 1.6m/s, 22 ℃ of wind-warm syndrome, humidity 42%; Ring blowing highly be 0.9m, cools off boundling afterwards, obtains moisture and be 18% polyvinyl alcohol as-spun fibre.
Embodiment 9
With the polyvinyl alcohol of the degree of polymerization 1700, alcoholysis degree 88%, molecular weight be 200 polyethylene glycol and water under stirring action in closed container swelling, wherein water accounts for 45% of three's gross mass, polyethylene glycol accounts for 8% of three's gross mass.Fully the polyvinyl alcohol after the swelling is used the double screw extruder spinning, and melt sprays from spinnerets, through ring blowing cooling; Wind speed 1m/s, 25 ℃ of wind-warm syndrome, humidity 45%; Ring blowing highly be 0.9m, cools off boundling afterwards, obtains moisture and be 21% polyvinyl alcohol as-spun fibre.
Embodiment 10
With the polyvinyl alcohol of the degree of polymerization 2000, alcoholysis degree 99%, molecular weight be 2000 polyethylene glycol and water under stirring action in closed container swelling, wherein water accounts for 45% of three's gross mass, polyethylene glycol accounts for 10% of three's gross mass.Fully the polyvinyl alcohol after the swelling is used the double screw extruder spinning, and melt sprays from spinnerets, through ring blowing cooling; Wind speed 2m/s, 20 ℃ of wind-warm syndrome, humidity 52%; Ring blowing highly be 0.6m, cools off boundling afterwards, obtains moisture and be 27% polyvinyl alcohol as-spun fibre.
Embodiment 11
With the polyvinyl alcohol of the degree of polymerization 1700, alcoholysis degree 92%, molecular weight be 1000 polyethylene glycol and water under stirring action in closed container swelling, wherein water accounts for 45% of three's gross mass, polyethylene glycol accounts for 10% of three's gross mass.Fully the polyvinyl alcohol after the swelling is used the double screw extruder spinning, and melt sprays from spinnerets, through ring blowing cooling; Wind speed 1.6m/s, 21 ℃ of wind-warm syndrome, humidity 50%; Ring blowing highly be 1m, cools off boundling afterwards, obtains moisture and be 24% polyvinyl alcohol as-spun fibre.
Embodiment 12
With the polyvinyl alcohol of the degree of polymerization 2600, alcoholysis degree 99%, monoethanolamine and water under stirring action in closed container swelling, wherein water accounts for 40% of three's gross mass, monoethanolamine accounts for 17% of three's gross mass.Fully the polyvinyl alcohol after the swelling is used the double screw extruder spinning, and melt sprays from spinnerets, through ring blowing cooling; Wind speed 1.5m/s, 24 ℃ of wind-warm syndrome, humidity 48%; Ring blowing highly be 0.8m, cools off boundling afterwards, obtains moisture and be 18% polyvinyl alcohol as-spun fibre.
Embodiment 13
With the polyvinyl alcohol of the degree of polymerization 2400, alcoholysis degree 99%, ethylene thiourea and water under stirring action in closed container swelling, wherein water accounts for 50% of three's gross mass, ethylene thiourea accounts for 5% of three's gross mass.Fully the polyvinyl alcohol after the swelling is used the double screw extruder spinning, and melt sprays from spinnerets, through ring blowing cooling; Wind speed 1.3m/s, 22 ℃ of wind-warm syndrome, humidity 43%; Ring blowing highly be 1.1m, cools off boundling afterwards, obtains moisture and be 22% polyvinyl alcohol as-spun fibre.
Embodiment 14
With the polyvinyl alcohol of the degree of polymerization 1700, alcoholysis degree 99%, citric acid and water under stirring action in closed container swelling, wherein water accounts for 55% of three's gross mass, citric acid accounts for 3% of three's gross mass.Fully the polyvinyl alcohol after the swelling is used the double screw extruder spinning, and melt sprays from spinnerets, through ring blowing cooling; Wind speed 1.7m/s, 20 ℃ of wind-warm syndrome, humidity 48%; Ring blowing highly be 0.7m, cools off boundling afterwards, obtains moisture and be 28% polyvinyl alcohol as-spun fibre.
Embodiment 15
With the polyvinyl alcohol of the degree of polymerization 2000, alcoholysis degree 99%, tartaric acid and water under stirring action in closed container swelling, wherein water accounts for 50% of three's gross mass, tartaric acid accounts for 6% of three's gross mass.Fully the polyvinyl alcohol after the swelling is used the double screw extruder spinning, and melt sprays from spinnerets, through ring blowing cooling; Wind speed 0.9m/s, 24 ℃ of wind-warm syndrome, humidity 50%; Ring blowing highly be 0.7m, cools off boundling afterwards, obtains moisture and be 24% polyvinyl alcohol as-spun fibre.
Claims (10)
1. ring blowing cooled and solidified process for preparing vinal, the polyvinyl alcohol melt is extruded from spinnerets, boundling behind blowing cooling formation as-spun fibre; It is characterized in that: the mode of ring blowing is adopted in described blowing cooling; The blowing of described ring is annular horizontal blowing cooling, promptly cools off air and flows perpendicular to the strand traffic direction and around tow, blow to strand, and technological parameter is: wind speed 0.6～3.5m/s; 21～25 ℃ of wind-warm syndrome, humidity 30～55%; Described polyvinyl alcohol melt is meant with water to be the molten polyethylene alcohol of plasticizer; The described polyvinyl alcohol degree of polymerization is 1500～2600, and alcoholysis degree is 88～99%.
2. a kind of ring blowing cooled and solidified process for preparing vinal according to claim 1 is characterized in that described ring blowing highly is 0.3～1.8m.
3. a kind of ring blowing cooled and solidified process for preparing vinal according to claim 1 is characterized in that the moisture of described polyvinyl alcohol melt is 30～60wt%.
4. according to claim 1 or 3 described a kind of ring blowing cooled and solidified processes that prepare vinal; It is characterized in that, also comprise the compound that can form hydrogen bond that accounts for polyvinyl alcohol melt gross mass 1～20wt% in the described polyvinyl alcohol melt with the hydroxyl in the polyvinyl alcohol.
5. a kind of ring blowing cooled and solidified process for preparing vinal according to claim 4; It is characterized in that the described compound that can form hydrogen bond with the hydroxyl in the polyvinyl alcohol is nitrogen-containing compound, hydroxy-containing compounds, sulfur-containing compound or carboxylated compound.
6. a kind of ring blowing cooled and solidified process for preparing vinal according to claim 5 is characterized in that described nitrogen-containing compound is caprolactam, polyamide or aqueous polyurethane; Hydroxy-containing compounds is that glycerine, monoethanolamine or molecular weight are 200～2000 polyethylene glycol; Sulfur-containing compound is an ethylene thiourea; Carboxylated compound is citric acid or tartaric acid.
7. a kind of ring blowing cooled and solidified process for preparing vinal according to claim 1 is characterized in that described wind speed is 1.5m/s.
8. a kind of ring blowing cooled and solidified process for preparing vinal according to claim 1 is characterized in that described wind-warm syndrome is 23 ℃.
9. a kind of ring blowing cooled and solidified process for preparing vinal according to claim 1 is characterized in that described cooling air humidity is 45%.
10. a kind of ring blowing cooled and solidified process for preparing vinal according to claim 1 is characterized in that described as-spun fibre moisture is 15～40wt%.
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| CN201210078774.7A CN102605446B (en) | 2012-03-22 | 2012-03-22 | Annular blowing cooling solidification process method for preparing polyvinyl alcohol fibre |
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| CN201210078774.7A CN102605446B (en) | 2012-03-22 | 2012-03-22 | Annular blowing cooling solidification process method for preparing polyvinyl alcohol fibre |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103866406A (en) * | 2013-10-30 | 2014-06-18 | 苏州龙杰特种纤维股份有限公司 | Monofilament stepped cooling method |
| CN104480550A (en) * | 2014-09-24 | 2015-04-01 | 江苏埃塞启航新材料装备制造有限公司 | Hollow polyphenylene sulfite short fiber multistage ring air-cooling process |
| CN109248505A (en) * | 2018-11-02 | 2019-01-22 | 宁波大发化纤有限公司 | A kind of regeneration chemical fibre circular blow system off gas circulation emission reduction device and its technique |
| CN113062004A (en) * | 2021-05-13 | 2021-07-02 | 永安市宝华林实业发展有限公司 | Method for preparing polyvinyl alcohol fiber by semi-molten wet method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103866406A (en) * | 2013-10-30 | 2014-06-18 | 苏州龙杰特种纤维股份有限公司 | Monofilament stepped cooling method |
| CN104480550A (en) * | 2014-09-24 | 2015-04-01 | 江苏埃塞启航新材料装备制造有限公司 | Hollow polyphenylene sulfite short fiber multistage ring air-cooling process |
| CN109248505A (en) * | 2018-11-02 | 2019-01-22 | 宁波大发化纤有限公司 | A kind of regeneration chemical fibre circular blow system off gas circulation emission reduction device and its technique |
| CN113062004A (en) * | 2021-05-13 | 2021-07-02 | 永安市宝华林实业发展有限公司 | Method for preparing polyvinyl alcohol fiber by semi-molten wet method |
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