CN101792938A - Novel preparation technology of polyoxymethylene fiber - Google Patents

Novel preparation technology of polyoxymethylene fiber Download PDF

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CN101792938A
CN101792938A CN 201010137926 CN201010137926A CN101792938A CN 101792938 A CN101792938 A CN 101792938A CN 201010137926 CN201010137926 CN 201010137926 CN 201010137926 A CN201010137926 A CN 201010137926A CN 101792938 A CN101792938 A CN 101792938A
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slow cooling
temperature
fiber
preparation technology
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CN101792938B (en
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倪建华
王依民
文珍稀
陈兴福
王艳萍
戴东鹏
王琳
夏于旻
陆燕飞
冯强
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JIANGSU YONGYIN CHEMICAL FIBER CO Ltd
Donghua University
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JIANGSU YONGYIN CHEMICAL FIBER CO Ltd
Donghua University
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Abstract

The invention relates to a novel preparation technology of polyoxymethylene fiber, in particular to the novel preparation technology of the polyoxymethylene fiber via multi-stage slow cooling and three-stage drawing with different media, which comprises the following steps: vacuum-drying polyoxymethylene granular materials, heating and melting via a screw extruder, melting and extruding by a spinneret, leading small melt flow to pass through the multi-stage slow cooling, carrying out high-speed traction, passing through a moistening and oiling cluster, winding, then obtaining as-spun fiber, carrying out hot air drawing and two times of drawing with different types of solvent, then carrying out hot molding and finally preparing the polyoxymethylene fiber. The novel prepration technology can solve the problems of matching between the multiple sections of atmosphere and temperature and the spinning process control and the control of the drawing with multiple media and make up for the deficiencies that the single atmosphere and temperature and the single medium drawing of the prior art lead the structure to be difficult to stable and uniform.

Description

A kind of novel preparation technology of polyformaldehyde fibre
Technical field
The present invention relates to a kind of novel preparation technology of polyformaldehyde fibre, particularly relate to a kind of novel preparation technology of the polyformaldehyde fibre that stretches through multistage slow cooling and three grades of different mediums.
Background technology
Polyformaldehyde (POM) is the fiber of a kind of high density, high crystalline, has the excellent comprehensive performance.Inherited most of advantage of polyformaldehyde and can give full play to the potential advantages of polyformaldehyde by the polyformaldehyde fibre of polyformaldehyde preparation.Polyformaldehyde fibre has high rigidity, high-intensity characteristics; Also abrasion performance, DIMENSIONAL STABILITY are good for it, and good endurance can be used for a long time; Its chemical-resistant, especially alkali resistance excellence.
EP2006000118 discloses the method that a kind of production has the POM monofilament of excellent crooked recovery.This method comprises to be extruded the POM copolymer by the spinning head mould, the polymer filament of heat is cooled off by 150 ℃ liquid bath, is stretched to total drawing ratio through single or multiple subsequently and is no more than 6: 1; Its shortcoming is that aqueous solution spinning is a parallel spinning, and area of mill site is big, and spinning speed is slow, and production capacity is low, cost height, the fine footpath of monofilament irregularity height.
JP2002009517 discloses a kind of manufacture method with POM fiber of high strength, high elasticity modulus.This method mainly comprises the polyacetal copolymer that contains adjustable oxyalkylene repeat units in the preparation strand; With this polymer melt spinning, the melt of heat sprays from spinnerets, and filament draws at a high speed and is wound up on the roller by the heating of single atmosphere temperature the time, and the velocity ratio that rolls out roller and work beam by control makes the POM fiber of certain stretching ratio.The defective of this invention is the variation that can not adapt to deformation region velocity gradient under the plate, and the stability of the uniformity of fibre structure and performance is not enough.
Summary of the invention
The objective of the invention is to adopt a kind of novel preparation technology of polyformaldehyde fibre, can obtain production efficiency height, low, the even structure of cost, stay-in-grade POM fiber in order to improve the defective of above-mentioned technology.
The present invention has carried out positive exploration in order to reach above-mentioned purpose, the very big influence of stretching condition when heating condition when the POM high polymer molten sprayed when the uniformity of discovery fiber was subjected to spinning and after-drawing.
The present invention relates to a kind of POM high polymer is heated and make its slowly method of cooling, these heating means are the gradient-heated method, have promptly adopted multistage slow cooling (staged slow cooling) technology, make high polymer slowly cooling in stable heating environment, and carry out the high speed traction.The invention still further relates to a kind of drawing process of POM fiber, three grades of drawing process that the POM as-spun fibre stretches by hot-air stretching, water-bath stretching and oil bath successively in this drawing process, the degree of orientation of fiber and degree of crystallinity increase, and the fibre of fiber is directly evenly simultaneously.
The novel preparation technology of a kind of polyformaldehyde fibre of the present invention, with polyoxymethylene granulate vacuumize, through the screw extruder heating and melting, melt extrude by spinnerets, the melt thread is by secondary slow cooling at least and carry out the high speed traction, and through the dewing boundling that oils, the back of reeling obtains as-spun fibre, the stretching of as-spun fibre hot-air is stretched through the twice different solvents again, make polyformaldehyde fibre by HEAT SETTING again.
As optimized technical scheme:
The novel preparation technology of aforesaid a kind of polyformaldehyde fibre, wherein, the fusing point of described polyformaldehyde is not less than 140 ℃, and the vitrifying deformation temperature is not less than 80 ℃.
The novel preparation technology of aforesaid a kind of polyformaldehyde fibre, wherein, described vacuum drying temperature is 70~130 ℃, the time is 3~15 hours; Vacuum is-0.05~-0.1MPa.Baking temperature is lower than 70 ℃, drying time and is less than 3 hours, polyoxymethylene granulate can not intensive drying, and the POM fluid produced bubble when residual moisture can cause spinning, and these bubbles remain in the POM fibril, to make the back processing of fiber become difficult, performance also descends greatly; Baking temperature is higher than 130 ℃, and the POM polymer will partly decompose, and influences the machine-shaping of high polymer.
The novel preparation technology of aforesaid a kind of polyformaldehyde fibre, wherein, the extruder temperature of described screw extruder is respectively: feed zone is 50~180 ℃, the preheating zone is 160~210 ℃, melting zone is 180~250 ℃, and the compressional zone is 180~250 ℃, and metering zone is 180~250 ℃; Spinning manifold is 180~250 ℃.Temperature is low excessively, is lower than 160 ℃, then fully fusion of POM high polymer, and spinning process can not be carried out; Temperature is too high, is higher than 250 ℃, and then thermal degradation will take place the POM high polymer, just can occur bubble and molten drop phenomenon during spinning, and the spinning environment is abominable, and the back processability and the combination property of fiber will descend greatly.
The novel preparation technology of aforesaid a kind of polyformaldehyde fibre, wherein, the slow cooling of described secondary at least is the level Four slow cooling, comprising: the one-level slow cooling: the atmosphere temperature is 120~250 ℃, is distance 1~160mm under the spinnerets plate between the active region; The secondary slow cooling: the atmosphere temperature is 120~180 ℃, is distance 161~220mm under the spinnerets plate between the active region; Three grades of slow cooling: the atmosphere temperature is 100~180 ℃, is distance 221~280mm under the spinnerets plate between the active region; The level Four slow cooling: the atmosphere temperature is 60~105 ℃, is distance 281~450mm under the spinnerets plate between the active region.The atmosphere temperature of described secondary at least slow cooling is with reducing one by one from the following distance of spinnerets plate between the active region, and the atmosphere temperature of first order slow cooling should be approaching with the high polymer molten temperature, to reduce the extrusion swelling of melt, prevents melt fracture; The atmosphere temperature of the second level, the third level, fourth stage slow cooling is mainly between 60~180 ℃, be to change in high polymer molten temperature and the solidification temperature scope, can prolong the solidification rate of melt thread, improve jet stretch ratio, effectively slow down the crystallization rate of POM high polymer, make the Stability Analysis of Structures of as-spun fibre.
The novel preparation technology of aforesaid a kind of polyformaldehyde fibre, wherein, described winding speed is 50~5000m/min.
The novel preparation technology of aforesaid a kind of polyformaldehyde fibre, wherein, 4.0~11.5 times of the total multiplying powers of stretching that described hot-air stretches and the twice different solvents stretches; The stretching ratio 2.0~3.6 that described hot-air stretches, drawing medium is an air, 50~80 ℃ of draft temperatures; Described twice different solvents stretches and is followed successively by water-bath stretching and oil bath stretching, wherein, and the stretching ratio 1.2~2.2 that described water-bath stretches, drawing medium is a water, 65~95 ℃ of draft temperatures, the stretching ratio 1.02~1.6 that oil bath stretches, drawing medium is oil bath, 70~125 ℃ of draft temperatures.The medium order that the twice solvent stretches can not change because a key effect of aqueous medium is to spin finish before the flush away, spin before preventing finish with after spin finish (oil bath drawing medium) and mix, to after spin finish and exert an influence.
The novel preparation technology of aforesaid a kind of polyformaldehyde fibre, wherein, the temperature of described HEAT SETTING is 60~115 ℃, shaping time is 10~40 minutes.
The novel preparation technology of a kind of polyformaldehyde fibre of the present invention, basic principle are melt ejections in extruder type spinning machine, and filament is by multistage slow cooling, and first order heating reduces the extrusion swelling of melt, prevents the melt fracture phenomenon; Heat the second level, has prolonged the viscosity flow deformation time of melt thread, can carry out thin neck stretcher strain fully, improves jet stretch ratio effectively; The third level and fourth stage heating, solidifying balancing effect when solidifying for the melt thread provides advantage, can make that the internal stress that produces when thread solidifies obtains discharging, and internal flaw obtains repairing.By multistage annealing device heating, prolonged the solidification rate of melt thread greatly, the crystallization rate that can effectively slow down the POM high polymer improves jet stretch ratio, makes constitutionally stable as-spun fibre.As-spun fibre is carried out after-drawing handle, mainly adopt three grades of stretchings, the first order is stretching in the hot-air carries out, and can improve the orientation of fiber greatly and degree of crystallinity is unlikely to have too big variation; It is medium that water stretch to be adopted in the second level, spins finish before the flush away, is convenient to the carrying out that level stretches behind the fiber, and the existence of hydrone simultaneously makes fiber generation swelling phenomenon, reduces the internal stress of fiber, promotes macromolecular crystallization; The third level stretches and adopts finish is medium, easy temperature control, heat transfer rate is fast, can rapidly the POM fiber be heated to draft temperature and temperature fluctuation is little, can make level and smooth stable fiber, can improve the particular characteristic of fiber by in finish, adding different auxiliary agents or changing the auxiliary agent proportioning simultaneously, satisfy the needs of different product.
The invention has the beneficial effects as follows:
Adopt multistage annealing device, can effectively slow down the POM crystallization rate, improve jet stretch ratio, the fine footpath of gained as-spun fibre is very even, the generation of lousiness in the time of effectively reducing the after-drawing processing.
Respectively with the stretching of heating of hot-air, water and oil bath medium, help that POM fiber finer neck stretches evenly, make the stable mechanical property of fiber.The different media of heating is adopted in the different stretch zone, has both helped the even structure of tensile fiber refinement, can fuse different auxiliary agents again and handle, and improves the back processing characteristics of fiber.
The novel preparation technology of a kind of polyformaldehyde fibre of the present invention, even, the stable performance in the fine footpath of prepared fiber can be used for making screen cloth; Hawser; Silkworm gut, mesh bag; Low temperature material; Sporting goods; The reinforcing material of concrete, synthetic resin etc., the stiffener of cable etc.; The fields such as framework material of rubbers such as tire, conveyer belt and driving belt.
Description of drawings
Accompanying drawing is the process chart of the novel preparation technology of a kind of polyformaldehyde fibre of the present invention
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 and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
The process chart of the novel preparation technology of a kind of polyformaldehyde fibre of the present invention with reference to the accompanying drawings, embodiment is as follows:
Embodiment 1:
The melt index (MI) of being measured by ASTMD1238 is the POM pellet of 1.8g/10min, temperature be 115 ℃ of vacuums for the condition of-0.1MPa under dry 4.5 hours.Pellet is through the screw extruder heating and melting, and melt extruded the screw rod spinning temperature by spinnerets after the measuring pump metering: feed zone is 177 ℃, and the preheating zone is 219 ℃, and melting zone is 216 ℃, and the compressional zone is 217 ℃, and metering zone is 216 ℃; Spinning manifold is 216 ℃.The melt thread passes through the level Four slow cooling, annealing device: the one-level slow cooling, and the atmosphere temperature is 220 ℃, is spinnerets plate distance 1~160mm down between the active region; The secondary slow cooling, the atmosphere temperature is 175 ℃, is distance 161~220mm under the spinnerets plate between the active region; Three grades of slow cooling, the atmosphere temperature is 140 ℃, is distance 221~280mm under the spinnerets plate between the active region; The level Four slow cooling, the atmosphere temperature is 100 ℃, is distance 281~450mm under the spinnerets plate between the active region; And carry out high speed traction, and through the dewing boundling that oils, the back of reeling obtains as-spun fibre, and coiling speed is 3000m/min.To stretch through the twice different solvents after the stretching of as-spun fibre hot-air, first order hot-air draft temperature is 70 ℃ again, and stretching ratio is 3.4; Water-bath draft temperature in the second level is 80 ℃, and stretching ratio is 2; Third level oil bath draft temperature is 100 ℃, and stretching ratio is 1.4.The fiber that stretched is made polyformaldehyde fibre by HEAT SETTING again, and the temperature of HEAT SETTING is 90 ℃, and shaping time is 15 minutes.The uniformity of the POM fiber of gained is better, intensity and modulus height, stable performance.
Embodiment 2:
Other conditions such as embodiment 1 just change the annealing device temperature: one-level slow cooling, atmosphere temperature are 210 ℃; Secondary slow cooling, atmosphere temperature are 170 ℃; Three grades of slow cooling, atmosphere temperature are 130 ℃; Level Four slow cooling, atmosphere temperature are 90 ℃.Through twice different solvents stretch after the as-spun fibre hot-air is stretched this moment again, and first order hot-air stretches, and stretching ratio is 3.4; Second level water-bath stretches, and stretching ratio is 2; Third level oil bath stretches, and stretching ratio is 1.6.The uniformity of the POM fiber of gained is best, intensity and modulus height, stable performance.
Embodiment 3:
Other conditions such as embodiment 1 just change the annealing device temperature: one-level slow cooling, atmosphere temperature are 190 ℃; Secondary slow cooling, atmosphere temperature are 150 ℃; Three grades of slow cooling, atmosphere temperature are 100 ℃; Level Four slow cooling, atmosphere temperature are 80 ℃.Through twice different solvents stretch after the as-spun fibre hot-air is stretched this moment again, and first order hot-air stretches, and stretching ratio is 3.2; Second level water-bath stretches, and stretching ratio is 1.9; Third level oil bath stretches, and stretching ratio is 1.4.The uniformity of the POM fiber of gained is general, and intensity and modulus are not high, and performance is more stable.
Embodiment 4:
Other conditions such as embodiment 1 just change the annealing device temperature: one-level slow cooling, atmosphere temperature are 145 ℃; Secondary slow cooling, atmosphere temperature are 140 ℃; Three grades of slow cooling, atmosphere temperature are 100 ℃; Level Four slow cooling, atmosphere temperature are 80 ℃.Through twice different solvents stretch after the as-spun fibre hot-air is stretched this moment again, and first order hot-air stretches, and stretching ratio is 3.1; Second level water-bath stretches, and stretching ratio is 1.9; Third level oil bath stretches, and stretching ratio is 1.1.The lack of homogeneity of the POM fiber of gained, intensity and modulus are low, unstable properties.
Embodiment 5:
Other conditions such as embodiment 1, just changing annealing device is three grades of slow cooling: the one-level slow cooling, the atmosphere temperature is 210 ℃, is distance 1~160mm under the spinnerets plate between the active region; The secondary slow cooling, the atmosphere temperature is 160 ℃, is distance 161~220mm under the spinnerets plate between the active region; Three grades of slow cooling, the atmosphere temperature is 100 ℃, is distance 221~280mm under the spinnerets plate between the active region.Through twice different solvents stretch after the as-spun fibre hot-air is stretched this moment again, and first order hot-air draft temperature is 70 ℃, and stretching ratio is 3.3; Water-bath draft temperature in the second level is 80 ℃, and stretching ratio is 2; Third level oil bath draft temperature is 100 ℃, and stretching ratio is 1.45.The good uniformity of the POM fiber of gained, intensity and modulus height, performance is more stable.
Embodiment 6:
Other conditions such as embodiment 1, just changing annealing device is the secondary slow cooling: the one-level slow cooling, the atmosphere temperature is 210 ℃, is distance 1~160mm under the spinnerets plate between the active region; The secondary slow cooling, the atmosphere temperature is 140 ℃, is distance 161~220mm under the spinnerets plate between the active region; And carry out high speed traction, and through the dewing boundling that oils, the back of reeling obtains as-spun fibre, and coiling speed is 3000m/min.To stretch through the twice different solvents after the stretching of as-spun fibre hot-air, first order hot-air draft temperature is 70 ℃ again, and stretching ratio is 3.3; Water-bath draft temperature in the second level is 80 ℃, and stretching ratio is 2; Third level oil bath draft temperature is 100 ℃, and stretching ratio is 1.35.The uniformity of the POM fiber of gained is better, and intensity and modulus are higher, and performance is more stable.
Table 1 reflection be the influence of the progression of annealing device among the embodiment 1~6 and heating-up temperature thereof to the fracture strength and the modulus of fiber, therefrom be not difficult to find out: multistage slow cooling has certain influence to the stability of fiber, select the level Four slow cooling, the uniformity of fiber and stability are best.Slow cooling temperature at different levels also all have certain influence to the mechanical property of fiber, wherein the temperature of one-level slow cooling is selected with the spinnerets temperature approaching, the temperature of secondary slow cooling is more than the fusing point (160 ℃) of high polymer, the temperature of three grades of slow cooling is on the vitrifying deformation temperature, the temperature of level Four slow cooling is near the vitrifying deformation temperature, and the stretching ratio of fiber is the highest, and draw ratio is more abundant, fiber stable best, the structure of fiber is also very even.
Table 1
The embodiment numbering The one-level slow cooling (℃) The secondary slow cooling (℃) Three grades of slow cooling (℃) The level Four slow cooling (℃) Total stretching ratio Percentage elongation (%) Fracture strength (cN/dtex) Modulus (cN/dtex)
??1 ??220 ??175 ??140 ??100 ??9.5 ??25.5 ??6.3 ??50.3
??2 ??210 ??170 ??130 ??90 ??10.9 ??20.9 ??6.8 ??51.4
??3 ??190 ??150 ??100 ??80 ??8.8 ??30.1 ??5.5 ??43.2
??4 ??170 ??150 ??100 ??80 ??6.5 ??37.8 ??4.0 ??37.5
??5 ??210 ??160 ??100 ??※ ??9.6 ??24.9 ??6.3 ??50.8
??6 ??210 ??140 ??※ ??※ ??8.9 ??28.5 ??5.9 ??46.1
Embodiment 7:
The melt index (MI) of being measured by ASTMD1238 is the POM pellet of 1.8g/10min, temperature be 115 ℃ of vacuums for the condition of-0.1MPa under dry 4.5 hours.Pellet is through the screw extruder heating and melting, and melt extruded the screw rod spinning temperature by spinnerets: feed zone is 77 ℃, and the preheating zone is 219 ℃, and melting zone is 216 ℃, and the compressional zone is 217 ℃, and metering zone is 216 ℃; Spinning manifold is 216 ℃.The melt thread passes through the level Four slow cooling, annealing device: the one-level slow cooling, and the atmosphere temperature is 210 ℃, is spinnerets plate distance 1~160mm down between the active region; The secondary slow cooling, the atmosphere temperature is 170 ℃, is distance 161~220mm under the spinnerets plate between the active region; Three grades of slow cooling, the atmosphere temperature is 130 ℃, is distance 221~280mm under the spinnerets plate between the active region; The level Four slow cooling, the atmosphere temperature is 90 ℃, is distance 281~450mm under the spinnerets plate between the active region.And carry out high speed traction, and through the dewing boundling that oils, the back of reeling obtains as-spun fibre, and coiling speed is 3000m/min.To stretch through the twice different solvents after the stretching of as-spun fibre hot-air, first order hot-air draft temperature is 75 ℃ again, and stretching ratio is 3.6; Water-bath draft temperature in the second level is 90 ℃, and stretching ratio is 2.1; Third level oil bath draft temperature is 110 ℃, and stretching ratio is 1.42.The fiber that stretched is made polyformaldehyde fibre by HEAT SETTING again, and the temperature of HEAT SETTING is 90 ℃, and shaping time is 15 minutes.The uniformity of the POM fiber of gained is better, and intensity and modulus are lower, and performance is more stable.
Embodiment 8:
Other conditions such as embodiment 5 just change draft temperature: first order hot-air draft temperature is 70 ℃, and stretching ratio is 3.5; Water-bath draft temperature in the second level is 90 ℃, and stretching ratio is 2.1; Third level oil bath draft temperature is 100 ℃, and stretching ratio is 1.53.The uniformity of the POM fiber of gained is best, intensity and modulus height, stable performance.
Embodiment 9:
Other conditions such as embodiment 5 just change draft temperature: first order hot-air draft temperature is 60 ℃, and stretching ratio is 3.1; Water-bath draft temperature in the second level is 90 ℃, and stretching ratio is 2.2; Third level oil bath draft temperature is 100 ℃, and stretching ratio is 1.57.The good uniformity of the POM fiber of gained, intensity and modulus height, performance is more stable.
Embodiment 10:
Other conditions such as embodiment 5 just change draft temperature: first order hot-air draft temperature is 70 ℃, and stretching ratio is 3.4; Water-bath draft temperature in the second level is 80 ℃, and stretching ratio is 2; Third level oil bath draft temperature is 90 ℃, and stretching ratio is 1.31.The uniformity of the POM fiber of gained is general, and intensity and modulus are higher, and performance is more stable.
Embodiment 11:
Other conditions such as embodiment 5 just change draft temperature: first order hot-air draft temperature is 70 ℃, and stretching ratio is 3.5; Water-bath draft temperature in the second level is 80 ℃, and stretching ratio is 2; Third level oil bath draft temperature is 100 ℃, and stretching ratio is 1.5.The uniformity of the POM fiber of gained is better, intensity and modulus height, stable performance.
Embodiment 12:
Other conditions such as embodiment 5 just change draft temperature: first order hot-air draft temperature is 60 ℃, and stretching ratio is 3.1; Water-bath draft temperature in the second level is 70 ℃, and stretching ratio is 1.8; Third level oil bath draft temperature is 80 ℃, and stretching ratio is 1.22.The uniformity of the POM fiber of gained is relatively poor, and intensity and modulus are low, unstable properties.
Embodiment 13:
Other conditions such as embodiment 5 just change draft temperature: first order hot-air draft temperature is 50 ℃, and stretching ratio is 2.4; Water-bath draft temperature in the second level is 55 ℃, and stretching ratio is 1.5; Third level oil bath draft temperature is 65 ℃, and stretching ratio is 1.1.The lack of homogeneity of the POM fiber of gained, intensity and modulus are low, unstable properties.
Table 2 be among the embodiment 7~13 three grades of draft temperatures to the influence of the fracture strength and the modulus of fiber, reflect: draft temperatures at different levels are to the stretching ratio of fiber, and the influence of the mechanical property of fiber, wherein work as one-level hot-air draft temperature and be lower than 60 ℃, secondary water-bath draft temperature is lower than 70 ℃, three grades of oil bath draft temperatures are lower than 80 ℃ and all are unfavorable for the carrying out that stretch will causing the uniformity of fiber to be affected, and the performance of fiber can not get fully playing consistently simultaneously; Temperature is too high, and especially the temperature of third level oil bath stretching is too high, surpasses 110 ℃ high polymer is partly decomposed, and serious situation will make fiber fuse, and influence the performance of fiber.
Table 2
The embodiment numbering The one-level stretching (℃) Secondary drawing (℃) Three grades of stretchings (℃) Total stretching ratio Percentage elongation (%) Fracture strength (cN/dtex) Modulus (cN/dtex)
??7 ??75 ??90 ??110 ??10.7 ??19.3 ??5.9 ??33.5
??8 ??70 ??90 ??100 ??11.5 ??17.5 ??6.5 ??52.4
??9 ??60 ??90 ??100 ??10.3 ??21.6 ??6.1 ??47.0
??10 ??70 ??80 ??90 ??8.9 ??29.7 ??5.2 ??36.4
??11 ??70 ??80 ??100 ??10.5 ??22.0 ??6.3 ??49.7
??12 ??60 ??70 ??80 ??6.8 ??40.4 ??4.7 ??20.2
??13 ??50 ??55 ??65 ??4.0 ??45.2 ??3.6 ??12.7

Claims (5)

1. the novel preparation technology of a polyformaldehyde fibre, it is characterized in that: with polyoxymethylene granulate vacuumize, through the screw extruder heating and melting, melt extrude by spinnerets, the melt thread is by secondary slow cooling at least and carry out the high speed traction, and through the dewing boundling that oils, the back of reeling obtains as-spun fibre, with stretching through the twice different solvents again after the stretching of as-spun fibre hot-air, make polyformaldehyde fibre by HEAT SETTING again.
2. the novel preparation technology of a kind of polyformaldehyde fibre as claimed in claim 1 is characterized in that, described vacuum drying temperature is 70~130 ℃, 3~15 hours time; Vacuum is-0.05~-0.1MPa.
3. the novel preparation technology of a kind of polyformaldehyde fibre as claimed in claim 1 is characterized in that, the slow cooling of described secondary at least is the level Four slow cooling, comprising: the one-level slow cooling: the atmosphere temperature is 120~250 ℃, is distance 1~160mm under the spinnerets plate between the active region; The secondary slow cooling: the atmosphere temperature is 120~180 ℃, is distance 161~220mm under the spinnerets plate between the active region; Three grades of slow cooling: the atmosphere temperature is 100~180 ℃, is distance 221~280mm under the spinnerets plate between the active region; The level Four slow cooling: the atmosphere temperature is 60~105 ℃, is distance 281~450mm under the spinnerets plate between the active region.
4. the novel preparation technology of a kind of polyformaldehyde fibre as claimed in claim 1 is characterized in that, 4.0~11.5 times of the total multiplying powers of stretching that described hot-air stretches and the twice different solvents stretches; The stretching ratio 2.0~3.6 that described hot-air stretches, drawing medium is an air, 50~80 ℃ of draft temperatures; Described twice different solvents stretches and is followed successively by water-bath stretching and oil bath stretching, wherein, and the stretching ratio 1.2~2.2 that described water-bath stretches, drawing medium is a water, 65~95 ℃ of draft temperatures, the stretching ratio 1.02~1.6 that oil bath stretches, drawing medium is oil bath, 70~125 ℃ of draft temperatures.
5. the novel preparation technology of a kind of polyformaldehyde fibre as claimed in claim 1 is characterized in that, 60~115 ℃ of the temperature of described HEAT SETTING, shaping time 10~40 minutes.
CN2010101379267A 2010-04-01 2010-04-01 Novel preparation technology of polyoxymethylene fiber Expired - Fee Related CN101792938B (en)

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CN102011201A (en) * 2010-12-15 2011-04-13 四川省纺织科学研究院 Melt-spinning method for polyformaldehyde fibers
CN102787377A (en) * 2012-09-03 2012-11-21 江苏恒力化纤股份有限公司 Manufacturing method of safe airbag polyester industrial yarn
CN103526308A (en) * 2013-10-30 2014-01-22 苏州龙杰特种纤维股份有限公司 Spun yarn manufacturing method
CN103541027A (en) * 2013-10-30 2014-01-29 苏州龙杰特种纤维股份有限公司 Producing and processing device for industrial spinning
CN103756246A (en) * 2013-11-13 2014-04-30 云南云天化股份有限公司 Spinning-grade polyoxymethylene material and preparation method thereof
CN105177756A (en) * 2015-10-27 2015-12-23 开滦(集团)有限责任公司 Method for preparing polyformaldehyde nascent fibers
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CN107805850A (en) * 2017-10-16 2018-03-16 唐山开滦化工科技有限公司 A kind of high-strength and high-modulus polyformaldehyde fibre and preparation method thereof
CN107938019A (en) * 2017-10-16 2018-04-20 唐山开滦化工科技有限公司 A kind of one-step shaping preparation method of polyformaldehyde fibre
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CN111118645A (en) * 2020-01-03 2020-05-08 西安交通大学 Preparation method of ultrahigh-strength polyformaldehyde fiber
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