CN105177756A - Method for preparing polyformaldehyde nascent fibers - Google Patents
Method for preparing polyformaldehyde nascent fibers Download PDFInfo
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- CN105177756A CN105177756A CN201510706062.9A CN201510706062A CN105177756A CN 105177756 A CN105177756 A CN 105177756A CN 201510706062 A CN201510706062 A CN 201510706062A CN 105177756 A CN105177756 A CN 105177756A
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Abstract
The invention discloses a method for preparing polyformaldehyde nascent fibers. The method includes the specific steps that polyformaldehyde resin and a small amount of o-cresol formaldehyde epoxy resin are evenly mixed and then placed into a vacuum drying box to be dried; the dried mixed materials are heated and fused in a screw extruder; spinning is carried out through a spinning assembly, spun filaments pass through a stage-by-stage slow-cooling and shock-cooling device (please see a figure in the specification) and are naturally cooled, then oil applying clustering and winding are carried out, and the nascent fibers are obtained. By means of the preparing method, the crystallinity of polyformaldehyde is effectively inhibited, the crystallization speed of the polyformaldehyde is decreased, good spinnability is given to the polyformaldehyde resin, the defects of broken filaments, surface micropores and the like generated in the multi-rate stretching process of the fibers are reduced, finished fibers obtained after the nascent fibers are stored for a period of time and then subjected to hot-air slow pulling processing are excellent in performance, the implementing method is simple, and production cost is low.
Description
Technical field
The present invention relates to a kind of preparation method of polyformaldehyde as-spun fibre, specifically be the present invention utilize step by step slow cooling-chilling apparatus to reduce the blemish of the polyformaldehyde as-spun fibre of acquisition, and then obtained high-performance finished fiber.
Background technology
Polyformaldehyde has another name called polyacetals, and it is a kind of unbranched linear high polymer, and density is high, degree of crystallinity is high, satisfactory mechanical property, chemical resistance strong, has excellent combination property.Polyformaldehyde can be divided into acefal homopolymer and the large class of copolymerized methanal two according to the existing mode of production and molecular chain structure thereof.Acefal homopolymer is polymerized by metaformaldehyde, and preparation technology is simple, but its heat endurance is poor in a heated condition, processing temperature scope is narrower, be very easily decomposed into formaldehyde gas; And copolymerized methanal is polymerized by metaformaldehyde and a small amount of dioxolanes, the decomposition preventing polyformaldehyde is added due to dioxolanes, improve the heat endurance of copolymerized methanal, its processing temperature scope is increased, have wider range of application, copolymerized methanal portion is in the market more than 80%.
The fiber prepared by polyformaldehyde not only inherits the most advantage of acetal resin but also adds many new advantages: high strength, high-modulus, excellent DIMENSIONAL STABILITY, heat endurance, alkali resistance, chemical resistance, fast light, weather-proof, abrasion performance etc., have high industrial utility value, application prospect is good.But, the degree of crystallinity of polyformaldehyde is very high, crystallization rate is exceedingly fast, in heating process, fusing point Sum decomposition temperature is extremely close, temperature in spinning process controls careless slightly, the problem such as the structure of the decomposition of polyformaldehyde or polyformaldehyde as-spun fibre just can be caused uneven, thus affecting the various performances of finished fiber, these are the maximum limiting factors improving fibre property in polyformaldehyde fibre production process.CN102011210A discloses a kind of method of producing the polyformaldehyde fibre of high fracture strength, as-spun fibre is adopted to the processing method of slow cooling-quenching in hot solution or vapours in drawing process.CN101792938A discloses a kind of technology of preparing of the polyformaldehyde fibre stretched through multistage slow cooling and three grades of different mediums.CN1555430A is by having carried out suitable control to polyformaldehyde crystallization rate, the manufacture method of fiber is improved, or the combination of both, when making stretching, the generation of fibrillation internal pore is suppressed, thus the polyformaldehyde fibre of preparation high strength, elastic modulus.US-3608044A1 has set forth a kind of preparation method of high elasticity polyformaldehyde fibre, and the solid particle making degree of crystallinity high by special method for crystallising bears elastic deformation.Sample after melt spinning, through a kind of special heat-wet process to improve the elasticity of fiber.WO-2008001924 has set forth a kind of manufacture method of polyformaldehyde fibre, is obtained the polyformaldehyde fibre of high strength by the half hitch crystallization time of MOLECULE DESIGN control polyformaldehyde.Although the article report of existing part polyformaldehyde spinning at present, preparation process more complicated.Mostly use spinning-grade acetal resin simultaneously, its dioxolanes content is higher than common acetal resin content, and manufacture process more complicated, have the fibre-grade acetal resin of report to be produced by Polyplastics at present, the more common acetal resin of price is high a lot.Add that existing production process is too complicated, production floor space is excessive, makes a lot of report all be only limited to laboratory primary stage or ideal phase, suitability for industrialized production can not be applied to further or in commercial process cost higher.
Summary of the invention
For the spinning-grade special raw material high cost existed in current polyformaldehyde fibre preparation process, the shortcoming of fiber manufacturing process complexity, the present invention with common polyformaldehyde for spinning material, by after it is mixed with a small amount of o-cresol formaldehyde epoxy resin as spinning material, be aided with slow cooling-chilling apparatus step by step simultaneously, restrained effectively the crystallinity of polyformaldehyde and reduce its crystalline rate, improve the defect on its crystal property, impart the spinnability that acetal resin is good, decrease the defect such as lousiness and surface micropore produced in fiber many multiplying powers drawing process, delay the finished fiber drawing process available energy excellent through hot-air after a period of time placed by the as-spun fibre obtained, its fracture strength can reach 0.8GPa, Young's modulus can reach 7.0GPa.
The present invention utilizes common acetal resin to prepare polyformaldehyde as-spun fibre, and relative to low price spinning-grade polyformaldehyde, abundant raw material source, preparation process is simple, greatly can reduce the production cost of spinning.It is at 190 DEG C, and under load 2160g condition, melt index is 11 ~ 27g/10min, and fusing point is about 155 ~ 175 DEG C, and construction unit is:
wherein: n, m be all be greater than 1 natural number.But the degree of crystallinity of polyformaldehyde is very high, and crystallization rate is exceedingly fast, especially common acetal resin, to successfully realize its spinnability and obtaining high performance finished fiber, effective ways must be adopted to reduce its crystallization rate and degree of crystallinity, reduce the blemish of as-spun fibre.The present invention adopt add in acetal resin mass percent be the o-cresol formaldehyde epoxy resin of 0.5 ~ 1.0% to disturb the method for its molecular chain movement to suppress its crystallization, to reduce its crystalline rate, spherulite size when simultaneously reducing polyformaldehyde crystallization improves the spinnability of common polyformaldehyde.In the present invention, o-cresol formaldehyde epoxy resin used is produced by Ba Ling petrochemical industry Co., Ltd, and its trade mark is CYDCN-2200, and number-average molecular weight is 550 ~ 1000, chemical constitution following (formula to be n be greater than 1 natural number):
When the present invention utilizes common polyformaldehyde to prepare polyformaldehyde as-spun fibre, its technical process comprises: mixing acetal resin raw material drying, heating and melting, filtration, measuring pump, filament spinning component, spinnerets, step by step slow cooling-quenching, the boundling that oils, winding.
Concrete processing step is as follows:
The first step: add the o-cresol formaldehyde epoxy resin that mass fraction is 0.5 ~ 1.0% in acetal resin, is positioned over dry 3-6h in the vacuum drying chamber of 90 ~ 110 DEG C after mixing;
Second step: dried mixed material is added in screw extruder and carries out heating and melting, screw extruder each district melt temperature is set as: 50 ~ 75 DEG C, a district, two 170 ~ 210 DEG C, districts, three 170 ~ 230 DEG C, districts, head 170 ~ 230 DEG C, assembly 200 ~ 235 DEG C;
3rd step: the polyformaldehyde melt after heating and melting after filtration, be evenly distributed in the spinneret orifice of filament spinning component and spray after metering, again through slow cooling-chilling apparatus and naturally cool fiber is cooled to 20-40 DEG C after to oil boundling, under winding speed is 300 ~ 1500m/min, receives silk, obtains polyformaldehyde as-spun fibre.
In the present invention, each district melt temperature setting value of screw extruder is: 50 ~ 75 DEG C, a district, two 170 ~ 210 DEG C, districts, three 170 ~ 230 DEG C, districts, head 170 ~ 230 DEG C, assembly 200 ~ 235 DEG C.In said temperature range of set value, when temperature is higher, the various aspects of performance of melt all can be higher, and therefore in setting range, temperature should raise as far as possible.If but temperature is too high, then melt can be made to degrade, the gas of generation can cause screw pressure to reduce or occur fluctuation, the fibre number of ejection is uneven, in discontinuous shape, even there will be bubble, make the aft-loaded airfoil difficulty of fiber, also greatly reduce the various aspects of performance of fiber simultaneously; If temperature is too low, then melt viscosity is too high, poor fluidity, and melt shear stress in spinneret orifice is excessive, causes melt fracture, and then affects its spinnability.
In the present invention, melt needs through at least three grades of slow cooling-quenchings after spinnerets ejection, and slow cooling adopts heating mantle heats air assembly, and quenching adopts cross air blowing device, its shape similar " ring ", and we name it to be slow cooling-chilling apparatus step by step in the present invention.
Further, slow cooling step by step-chilling apparatus total length is the 1/3-2/3 of spinnerets apart from the total distance of oiling device.
Further, wherein one-level slow cooling heating jacket upper surface is 0mm apart from spinnerets lower surface distance, and heating jacket length is 41% of slow cooling-chilling apparatus overall length, and heating-up temperature is 150 ~ 235 DEG C; Secondary slow cooling heating jacket upper surface is 45% of slow cooling-chilling apparatus overall length apart from spinnerets lower surface distance, and heating jacket length is 31% of slow cooling-chilling apparatus overall length, and heating-up temperature is 100 ~ 220 DEG C; Three grades of slow cooling heating jacket upper surfaces are 80% of slow cooling-chilling apparatus overall length apart from spinnerets lower surface distance, and heating jacket length is 20% of slow cooling-chilling apparatus overall length, and heating-up temperature is 70 ~ 160 DEG C.Quench length at different levels is 4% of slow cooling-chilling apparatus overall length,
Further, adopt cross air blowing device, wind-warm syndrome is 15-50 DEG C, and wind speed is 0.25 ~ 0.30m/s.Crystalline size and crystallization rate when reducing polyformaldehyde melt cooling by multistage slow cooling-quenching, crystal property is well controlled, and fibre structure also becomes stable, and the defects such as the lousiness produced in after-drawing process or micropore reduce.The length of heating jacket shortens with the increase of slow cooling-quenching progression, and heating-up temperature reduces with the increase of slow cooling-quenching progression, can while crystallization control speed and degree of crystallinity, make melt stream solidify gradually like this, forms the as-spun fibre that defect is few.
Further, slow cooling step by step-chilling apparatus lower end is nature cooling zone to oiling device interval, and temperature is room temperature, calm.
In the present invention, as-spun fibre reels and receives silk after the boundling that oils, and winding speed is 300 ~ 1500m/min, and best winding speed is 900 ~ 1200m/mim.Winding speed affects the pre-orientation degree of fiber, when winding speed is higher, pre-orientation degree is also higher, and in after-drawing process, draw ratio is then lower, but in production process under the prerequisite not affecting fiber quality for enhancing productivity, then winding speed should be high as far as possible.
As-spun fibre is obtained by the present invention, needing as-spun fibre to be placed on temperature before making finished fiber is 25 DEG C, humidity is 4 ~ 12h under the condition of 60% ~ 80%, it is 60 ~ 160 DEG C at draft temperature, stretching ratio is 6.0 ~ 10.0 times, winding speed is under 10 ~ 50m/min, obtains finished fiber through multistage stretching.Because melt is through spinning pack in spinning process, cause fiber that sharply deformation occurs thus make as-spun fibre inside produce internal stress, structure extremely unstable, fibre number not only can be made uneven if now stretch immediately, also can produce lousiness and broken end, therefore need as-spun fibre to place certain hour under certain condition, its internal stress is made to reduce even to disappear, in after-drawing process, make fibre structure become stable, fiber number is even, is conducive to stretching.
Main feature of the present invention is summarized as follows: what 1. polyformaldehyde raw material adopted is common polyformaldehyde but not spinning-grade polyformaldehyde, greatly reduces production cost, also makes spinning process and distinguishes to some extent in the past; 2. molecular chain movement time by adding a small amount of o-cresol formaldehyde epoxy resin and suppressing polyformaldehyde melt cooling and the size of crystalline size, make the fault of construction produced in the winding of fiber and after-drawing process reduce; 3. crystal property when installing slow cooling-chilling apparatus suppression polyformaldehyde melt cooling and crystalline size is passed through below spinnerets, spinneret draft is raised, and then obtain the uniform as-spun fibre of fiber number, reduce the generation probability of lousiness and fracture of wire in aft-loaded airfoil process.
Polyformaldehyde as-spun fibre obtained by the present invention, the superior polyformaldehyde finished fiber of availability after placing, delay and drawing, as: high strength, high-modulus, excellent DIMENSIONAL STABILITY, heat endurance, alkali resistance, chemical resistance, fast light, weather-proof, abrasion performance etc., add the feature that fiber itself has, it is made to have many uses, as the rope of cable car, concrete enhancing, industrial brush, canvas, the production field such as fishing net and life, industry and ocean.
Example will be listed below be specifically described the present invention.Example cited is below all individual example, not only embodiment.Change in all scope of the invention or in equivalent scope of the present invention is all included in the invention.
Accompanying drawing explanation
Fig. 1 is slow cooling-chilling apparatus in the present invention
Detailed description of the invention
Embodiment 1:
Acetal resin melt index is 11g/10min, and the mass percent that o-cresol formaldehyde epoxy resin adds is 1.0wt.%, by its dry 6h under 90 DEG C of conditions.Resin granular material, through screw extruder melting heating, is sprayed through spinnerets after being distributed, screw rod melt spinning each section of temperature: 60 DEG C, a district, two 210 DEG C, districts, three 200 DEG C, districts, head 230 DEG C, assembly 235 DEG C by measuring pump metering.Through slow cooling-chilling apparatus after melt stream sprays from spinnerets, slow cooling step by step-chilling apparatus total length is that spinnerets is apart from 1/3 of the total distance of oiling device, wherein one-level slow cooling heating jacket upper surface is 0mm apart from spinnerets lower surface distance, and heating jacket length is 200mm, and heating-up temperature is 235 DEG C; Secondary slow cooling heating jacket upper surface is 220mm apart from spinnerets lower surface distance, and heating jacket length is 150mm, and heating-up temperature is 220 DEG C; Three grades of slow cooling heating jacket upper surfaces are 390mm apart from spinnerets lower surface distance, and heating jacket length is 100mm, and heating-up temperature is 160 DEG C.Quench portion adopts lateral blowing cooling, and lateral blowing temperature is 50 DEG C, and wind speed is 0.3m/s.After fiber being cooled to 40 DEG C after naturally cooling again, after the boundling that oils, winding obtains as-spun fibre, and winding speed is 1200m/min.As-spun fibre is placed on temperature 25 DEG C, humidity is under the condition of 80% after 12h, and by slow drawing device at winding speed 20m/min, temperature is that stretching ratio is 8.0 through 4 grades of stretchings under the condition of 150 DEG C, obtained finished fiber.Its fracture strength is 0.68GPa, and Young's modulus is 5.9GPa.
Embodiment 2:
Acetal resin melt index is 11g/10min, and the mass percent that o-cresol formaldehyde epoxy resin adds is 1.0wt.%, by its dry 6h under 90 DEG C of conditions.Resin granular material, through screw extruder melting heating, is sprayed through spinnerets after being distributed, screw rod melt spinning each section of temperature: 60 DEG C, a district, two 210 DEG C, districts, three 200 DEG C, districts, head 230 DEG C, assembly 235 DEG C by measuring pump metering.Through slow cooling-chilling apparatus after melt stream sprays from spinnerets, slow cooling step by step-chilling apparatus total length is that spinnerets is apart from 1/3 of the total distance of oiling device, wherein one-level slow cooling heating jacket upper surface is 0mm apart from spinnerets lower surface distance, and heating jacket length is 200mm, and heating-up temperature is 235 DEG C; Secondary slow cooling heating jacket upper surface is 220mm apart from spinnerets lower surface distance, and heating jacket length is 150mm, and heating-up temperature is 220 DEG C; Three grades of slow cooling heating jacket upper surfaces are 390mm apart from spinnerets lower surface distance, and heating jacket length is 100mm, and heating-up temperature is 160 DEG C.Quench portion adopts lateral blowing cooling, and lateral blowing temperature is 50 DEG C, and wind speed is 0.3m/s.After fiber being cooled to 20 DEG C after naturally cooling again, after the boundling that oils, winding obtains as-spun fibre, and winding speed is 1200m/min.The as-spun fibre obtained is by slow drawing device at winding speed 20m/min, and temperature is that stretching ratio is 8.0 through 4 grades of stretchings under the condition of 150 DEG C, obtained finished fiber.Its fracture strength is 0.55GPa, and Young's modulus is 5.1GPa, and fracture of wire is very serious.
Embodiment 3:
Acetal resin melt index is 11g/10min, and the mass percent that o-cresol formaldehyde epoxy resin adds is 1.0wt.%, by its dry 6h under 90 DEG C of conditions.Resin granular material, through screw extruder melting heating, is sprayed through spinnerets after being distributed, screw rod melt spinning each section of temperature: 60 DEG C, a district, two 210 DEG C, districts, three 200 DEG C, districts, head 210 DEG C, assembly 220 DEG C by measuring pump metering.Through slow cooling-chilling apparatus after melt stream sprays from spinnerets, slow cooling step by step-chilling apparatus total length is that spinnerets is apart from 1/3 of the total distance of oiling device, wherein one-level slow cooling heating jacket upper surface is 0mm apart from spinnerets lower surface distance, and heating jacket length is 200mm, and heating-up temperature is 220 DEG C; Secondary slow cooling heating jacket upper surface is 220mm apart from spinnerets lower surface distance, and heating jacket length is 150mm, and heating-up temperature is 180 DEG C; Three grades of slow cooling heating jacket upper surfaces are 390mm apart from spinnerets lower surface distance, and heating jacket length is 100mm, and heating-up temperature is 160 DEG C.Quench portion adopts lateral blowing cooling, and lateral blowing temperature is 50 DEG C, and wind speed is 0.3m/s.After fiber being cooled to 30 DEG C after naturally cooling again, after the boundling that oils, winding obtains as-spun fibre, and winding speed is 1200m/min.As-spun fibre is placed on temperature 25 DEG C, humidity is under the condition of 80% after 12h, and by slow drawing device at winding speed 20m/min, temperature is that stretching ratio is 10.0 through 4 grades of stretchings under the condition of 150 DEG C, obtained finished fiber.Its fracture strength is 0.8GPa, and Young's modulus is 7.0GPa.
Embodiment 4:
Acetal resin melt index is 27g/10min, and the mass percent that o-cresol formaldehyde epoxy resin adds is 1.0wt.%, by its dry 3h under 110 DEG C of conditions.Resin granular material, through screw extruder melting heating, is sprayed through spinnerets after being distributed, screw rod melt spinning each section of temperature: 60 DEG C, a district, two 170 DEG C, districts, three 200 DEG C, districts, head 220 DEG C, assembly 230 DEG C by measuring pump metering.Through slow cooling-chilling apparatus after melt stream sprays from spinnerets, slow cooling step by step-chilling apparatus total length is that spinnerets is apart from 2/3 of the total distance of oiling device, wherein one-level slow cooling heating jacket upper surface is 0mm apart from spinnerets lower surface distance, and heating jacket length is 200mm, and heating-up temperature is 230 DEG C; Secondary slow cooling heating jacket upper surface is 220mm apart from spinnerets lower surface distance, and heating jacket length is 150mm, and heating-up temperature is 180 DEG C; Three grades of slow cooling heating jacket upper surfaces are 390mm apart from spinnerets lower surface distance, and heating jacket length is 100mm, and heating-up temperature is 160 DEG C.Quench portion adopts lateral blowing cooling, and lateral blowing temperature is 25 DEG C, and wind speed is 0.25m/s.After fiber being cooled to 30 DEG C after naturally cooling again, after the boundling that oils, winding obtains as-spun fibre, and winding speed is 800m/min.As-spun fibre is placed on temperature 25 DEG C, humidity is under the condition of 80% after 12h, and by slow drawing device at winding speed 50m/min, temperature is that stretching ratio is 6.0 through 4 grades of stretchings under the condition of 120 DEG C, obtained finished fiber.Its fracture strength is 0.45GPa, and Young's modulus is 4.8GPa.
Embodiment 5:
Acetal resin melt index is 27g/10min, and the mass percent that o-cresol formaldehyde epoxy resin adds is 1.0wt.%, by its dry 3h under 110 DEG C of conditions.Resin granular material, through screw extruder melting heating, is sprayed through spinnerets after being distributed, screw rod melt spinning each section of temperature: 60 DEG C, a district, two 170 DEG C, districts, three 200 DEG C, districts, head 220 DEG C, assembly 230 DEG C by measuring pump metering.Through slow cooling-chilling apparatus after melt stream sprays from spinnerets, slow cooling step by step-chilling apparatus total length is that spinnerets is apart from 2/3 of the total distance of oiling device, wherein one-level slow cooling heating jacket upper surface is 0mm apart from spinnerets lower surface distance, and heating jacket length is 200mm, and heating-up temperature is 230 DEG C; Secondary slow cooling heating jacket upper surface is 220mm apart from spinnerets lower surface distance, and heating jacket length is 150mm, and heating-up temperature is 180 DEG C; Three grades of slow cooling heating jacket upper surfaces are 390mm apart from spinnerets lower surface distance, and heating jacket length is 100mm, and heating-up temperature is 160 DEG C.Quench portion adopts lateral blowing cooling, and lateral blowing temperature is 25 DEG C, and wind speed is 0.25m/s.After fiber being cooled to 25 DEG C after naturally cooling again, after the boundling that oils, winding obtains as-spun fibre, and winding speed is 800m/min.As-spun fibre is placed on temperature 25 DEG C, humidity is under the condition of 80% after 12h, and by slow drawing device at winding speed 50m/min, temperature is that stretching ratio is 10.0 through 4 grades of stretchings under the condition of 120 DEG C, obtained finished fiber.Its fracture strength is 0.69GPa, and Young's modulus is 6.5GPa.
Embodiment 6:
Acetal resin melt index is 15g/10min, and the mass percent that o-cresol formaldehyde epoxy resin adds is 0.5wt.%, by its dry 3h under 110 DEG C of conditions.Resin granular material, through screw extruder melting heating, is sprayed through spinnerets after being distributed, screw rod melt spinning each section of temperature: 60 DEG C, a district, two 210 DEG C, districts, three 200 DEG C, districts, head 220 DEG C, assembly 200 DEG C by measuring pump metering.Through slow cooling-chilling apparatus after melt stream sprays from spinnerets, slow cooling step by step-chilling apparatus total length is that spinnerets is apart from 2/3 of the total distance of oiling device, wherein one-level slow cooling heating jacket upper surface is 0mm apart from spinnerets lower surface distance, and heating jacket length is 200mm, and heating-up temperature is 200 DEG C; Secondary slow cooling heating jacket upper surface is 220mm apart from spinnerets lower surface distance, and heating jacket length is 150mm, and heating-up temperature is 160 DEG C; Three grades of slow cooling heating jacket upper surfaces are 390mm apart from spinnerets lower surface distance, and heating jacket length is 100mm, and heating-up temperature is 100 DEG C.Quench portion adopts lateral blowing cooling, and lateral blowing temperature is 35 DEG C, and wind speed is 0.25m/s.After fiber being cooled to 30 DEG C after naturally cooling again, after the boundling that oils, winding obtains as-spun fibre, and winding speed is 1000m/min.As-spun fibre is placed on temperature 25 DEG C, humidity is under the condition of 80% after 12h, and by slow drawing device at winding speed 50m/min, temperature is that stretching ratio is 8.0 through 4 grades of stretchings under the condition of 120 DEG C, obtained finished fiber.Its fracture strength is 0.6GPa, and Young's modulus is 6.5GPa.
Embodiment 7:
Acetal resin melt index is 20g/10min, and the mass percent that o-cresol formaldehyde epoxy resin adds is 0.5wt.%, by its dry 3h under 110 DEG C of conditions.Resin granular material, through screw extruder melting heating, is sprayed through spinnerets after being distributed, screw rod melt spinning each section of temperature: 60 DEG C, a district, two 210 DEG C, districts, three 200 DEG C, districts, head 220 DEG C, assembly 200 DEG C by measuring pump metering.Through slow cooling-chilling apparatus after melt stream sprays from spinnerets, slow cooling step by step-chilling apparatus total length is that spinnerets is apart from 3/5 of the total distance of oiling device, wherein one-level slow cooling heating jacket upper surface is 0mm apart from spinnerets lower surface distance, and heating jacket length is 200mm, and heating-up temperature is 150 DEG C; Secondary slow cooling heating jacket upper surface is 220mm apart from spinnerets lower surface distance, and heating jacket length is 150mm, and heating-up temperature is 100 DEG C; Three grades of slow cooling heating jacket upper surfaces are 390mm apart from spinnerets lower surface distance, and heating jacket length is 100mm, and heating-up temperature is 70 DEG C.Quench portion adopts lateral blowing cooling, and lateral blowing temperature is 35 DEG C, and wind speed is 0.25m/s.After fiber being cooled to 30 DEG C after naturally cooling again, after the boundling that oils, winding obtains as-spun fibre, and winding speed is 1000m/min.As-spun fibre is placed on temperature 25 DEG C, humidity is under the condition of 80% after 12h, and by slow drawing device at winding speed 50m/min, temperature is that stretching ratio is 8.0 through 4 grades of stretchings under the condition of 120 DEG C, obtained finished fiber.Its fracture strength is 0.58GPa, and Young's modulus is 6.7GPa, and fracture of wire is more serious.
Claims (7)
1. the preparation method of a polyformaldehyde as-spun fibre, it is characterized in that: be that the acetal resin of 11 ~ 27g/10min mixes in the vacuum drying chamber being placed on 90 ~ 110 DEG C with a small amount of o-cresol formaldehyde epoxy resin and dries by melt index, by dried mixed material heating and melting in screw extruder, through filament spinning component spray silk, by slow cooling-chilling apparatus step by step, carry out through naturally cooling oil boundling, winding again, obtain polyformaldehyde as-spun fibre, concrete steps are as follows:
The first step: the o-cresol formaldehyde epoxy resin adding polyformaldehyde mass fraction 0.5 ~ 1.0% in acetal resin, is positioned over dry 3-6h in the vacuum drying chamber of 90 ~ 110 DEG C after mixing;
Second step: dried mixed material is added in screw extruder and carries out heating and melting, screw extruder each district melt temperature is set as: 50 ~ 75 DEG C, a district, two 170 ~ 210 DEG C, districts, three 170 ~ 230 DEG C, districts, head 170 ~ 230 DEG C, assembly 200 ~ 235 DEG C;
3rd step: the polyformaldehyde melt after heating and melting after filtration, be evenly distributed in the spinneret orifice of filament spinning component and spray after metering, again through slow cooling-chilling apparatus step by step with naturally cool fiber is cooled to 20-40 DEG C, then oil boundling, under winding speed is 300 ~ 1500m/min, receives silk, obtains polyformaldehyde as-spun fibre.
2. the preparation method of a kind of polyformaldehyde as-spun fibre according to claim 1, is characterized in that: melt is through three grades of slow cooling-quenching process after spinnerets ejection, and slow cooling adopts heating mantle heats air assembly, and quenching adopts cross air blowing device.
3. the preparation method of a kind of polyformaldehyde as-spun fibre according to claim 1, is characterized in that: slow cooling step by step-chilling apparatus total length is the 1/3-2/3 of spinnerets apart from the total distance of oiling device.
4. the preparation method of a kind of polyformaldehyde as-spun fibre according to claim 1, it is characterized in that: one-level slow cooling heating jacket upper surface is 0mm apart from spinnerets lower surface distance, heating jacket length is 41% of slow cooling-chilling apparatus overall length, and temperature is 150 ~ 235 DEG C; Secondary slow cooling heating jacket upper surface is 45% of slow cooling-chilling apparatus overall length apart from spinnerets lower surface distance, and heating jacket length is 31% of slow cooling-chilling apparatus overall length, and heating-up temperature is 100 ~ 220 DEG C; Three grades of slow cooling heating jacket upper surfaces are 80% of slow cooling-chilling apparatus overall length apart from spinnerets lower surface distance, and heating jacket length is 20% of slow cooling-chilling apparatus overall length, and heating-up temperature is 70 ~ 160 DEG C.
5. the preparation method of a kind of polyformaldehyde as-spun fibre according to claim 1, is characterized in that: adopt cross air blowing device, air temperature is 15-50 DEG C, and wind speed is 0.25 ~ 0.30m/s.
6. the preparation method of a kind of polyformaldehyde as-spun fibre according to claim 1, is characterized in that: slow cooling step by step-chilling apparatus lower end is nature cooling zone to oiling device interval, and temperature is room temperature, calm.
7. the application of polyformaldehyde as-spun fibre prepared of preparation method according to claim 1, it is characterized in that: polyformaldehyde as-spun fibre is 25 DEG C in temperature, humidity is the condition placement 4 ~ 12h of 60% ~ 80%, it is 60 ~ 160 DEG C at draft temperature, stretching ratio is 6.0 ~ 10.0 times, winding speed is under 10 ~ 50m/min, obtains finished fiber through multistage stretching.
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| CN115722209A (en) * | 2022-09-27 | 2023-03-03 | 东华大学 | Polyoxymethylene microfiber oil-water separation material and preparation method thereof |
| CN117137217A (en) * | 2023-08-29 | 2023-12-01 | 佛山市嘉颖内衣配件有限公司 | Underwear back buckle belt cloth pressing machine capable of automatically reducing temperature and enhancing bonding strength |
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