CN1180385A - Method of producing cellulose fibres - Google Patents

Method of producing cellulose fibres Download PDF

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Publication number
CN1180385A
CN1180385A CN 96192977 CN96192977A CN1180385A CN 1180385 A CN1180385 A CN 1180385A CN 96192977 CN96192977 CN 96192977 CN 96192977 A CN96192977 A CN 96192977A CN 1180385 A CN1180385 A CN 1180385A
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China
Prior art keywords
solidification
spinning solution
zone
technology
liquid
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CN 96192977
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Chinese (zh)
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G·弗里施马恩
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Akzo Nobel NV
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Akzo Nobel NV
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Priority to CN 96192977 priority Critical patent/CN1180385A/en
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Abstract

A process for manufacturing cellulose fibers by extrusion of a spinning solution, containing dissolved cellulose, into a gaseous medium through a predetermined gas zone, with subsequent immersion in and guidance through a coagulation bath over a predetermined coagulation zone, drawing the cellulose fibers obtained and winding them up, characterized in that after the gas zone the extruded spinning solution is immersed in a coagulation bath accelerated to a predetermined velocity and flowing laminarly at least approximately in the direction of the extruded spinning solution, whereby the coagulation liquid is fed laterally into the path of the spinning solution and the flow direction of the spinning solution and the coagulation liquid is kept approximately parallel throughout the entire coagulation zone, and in that the cellulose fibers obtained are laterally deflected upon leaving the coagulation zone and then wound up.

Description

Make the technology of cellulose fibre
The present invention relates to make the technology of cellulose fibre, the spinning of cellulose solution that contains dissolving by extruding enters in the gas phase media through a predetermined gas zone, immerse through a predetermined solidification zone then and guiding by coagulating bath, draw the cellulose fibre of gained and with its coiling.
For example from DE-A-4409609 this type of technology as can be known.Spinning solution is through immersing one fixedly in the coagulating bath behind the gas zone passage, coagulating bath is quickened together in company with spinning solution then.The acceleration of coagulating bath is undertaken by the spinning funnel that the bottom becomes taper to dwindle.The shortcoming of this kind spinning funnel is the spinning initial stage to produce a lot of problems.According to these embodiment, the winding speed of the maximum that can get is 150m/min, thereby this already known processes is not too economical.
Know another this type of technology from JP-A-6119805, wherein spinning solution also is extruded in the spinning funnel, because of the encapsulate effect of gas zone, the atmosphere that extrusion spinning solution enters is filled with a large amount of solidification liquids thus, causes the undesirable pre-solidification phenomenon of gas zone thus.In this already known processes, solidification liquid is introduced liquid stream through the spinning funnel wall, cause the just in time turbulent flow at contact point place between spinning solution and solidification liquid.This turbulent flow causes the interruption that spinning is frequent, has only with technology so far just to be directed at stable spinning process when using seldom spinning of cellulose solution.The winding speed that these embodiment provide is up to 1500m/min.But this is just reached by the several Accelerating funnels of arrangement, the cost costliness, and this at first causes the difficulty at spinning initial stage, and next makes stable spinning technique become more complicated significantly.
The objective of the invention is to carry out the new spinning technique of more economical produce cellulose fibers.Particularly should reduce above-mentioned shortcoming at least.The present invention also provides a kind of technology of produce cellulose fibers, when even it surpasses 1000m/min at winding speed, and use responsive cellulose spinning solution, for example having moisture tertiary amine N-oxide also is stable under the cellulose solution situation of N-methylmorpholine-N-oxide (NMMO) particularly.
The technology that this purpose was described by when beginning realizes, that is: after gas zone, the spinning solution that squeezes out is caused one to be accelerated in the solidification liquid of predetermined speed, and solidification liquid at least near the direction of the spinning solution that squeezes out with Laminar Flow, this moment, the solidification liquid side direction entered in the approach of spinning solution, and the flow direction of spinning solution and solidification liquid is at whole solidification zone keeping parallelism at least roughly, and when the gained cellulose fibre leaves solidification zone the side direction deflection, reel then.
The side direction laminar flow charging of solidification liquid can reach by following plain mode: make a side of solidification liquid storage tank form an overflow ducts, the shape of overflow ducts makes solidification liquid flow along outline line on the one hand, and makes it go to the flow direction of spinning solution from horizontal direction on the other hand.The shape of this outline line resembles 1/1st circle or parabola under the simple scenario, but should notice that the flow direction that goes to spinning solution from the overflow ducts outlet should form stable curve, to guarantee the no turbulent flow of the overwhelming majority, spinning solution can immerse in the laminar flow solidification liquid stream like this.Ideal method is to make overflow ducts still be parallel to the flow direction of spinning solution after turning to the flow direction of spinning solution, until the end of solidification zone, thereby the root edge that the coiler device that relies on the side direction biasing so as to the basal edge that utilizes overflow ducts is pulled through slinning cabinet with the tow that is produced makes the cellulose fibre deflection of generation.
Technology of the present invention is suitable for producd fibers, and the term fiber refers to monofilament, multifilament threads and air silk herein.This technology is suitable for producing porous fibre equally.These fibers can have cross section circular and abnormity.
Have 1.0 to 5mm the constant flow of liquid degree of depth if enter the solidification liquid of spinning solution from a side, then the production of the cellulose fibre that is undertaken by the present invention is successful especially.Particularly advantageous thus is to being about 1 to 3 times of the spinning solution maximum gauge extruded with the depth adjustment of liquid stream.The liquid flow depth degree that guarantees to have done the overflow ducts that is described in detail in the above is simple especially, wherein a certain amount of solidification liquid is delivered in the solidification liquid storage tank, thereby is formed the liquid flow depth degree that requires in the tangential exit of overflow ducts.Certainly, should be careful solidification liquid herein and enter in the storage tank with stable state at least, in storage tank, not cause turbulent flow.Those skilled in the art fully knows the device of this necessity, thereby need not be further explained in detail.
For technology of the present invention, the speed of recommended adjustment solidification liquid, so that immerse the velocity amplitude scope of putting at spinning solution is 30 to 200m/min, be preferably 50 to 80m/min, thereby if be 0.5 to 8cm with the length adjustment of solidification zone, when being preferably 1 to 4cm, the production of cellulose fibre is carried out good especially.
The speed that immerses the some place can be by the difference in height decision of the above technology that is described in detail by storage tank liquid level and spinning solution immersion point, and immersing point is the point that overflow ducts goes to the spinning solution flow direction.The speed that immerses the some place equals two times acceleration of gravity and the product square root of difference in height (speed square equal two times the acceleration of gravity and the product of difference in height).As the overflow ducts using, then be easy to partly determine solidification zone by the overflow ducts between the basal edge that immerses point and overflow ducts.
For in satisfied especially mode from the cellulose silk in solidification zone exit, removing solidification liquid, find that effective method is that to make the cellulose silk that solidifies after solidification zone be 45 to 60 ° for the deflection angle scope of the flow direction of solidification liquid.Recommend thus cellulose silk at the flow direction that departs from solidification liquid through sudden change ground after the solidification zone.Tu Bian the meaning fiber that is meant gained has only its direction of motion of change in several millimeters the zone very little in the present invention.This moment, to do like this be favourable, and the deflecting region radius that promptly makes the cellulose fibre sudden change ground of gained depart from the solidification liquid flow direction after solidification zone is 0.2 to 2mm, is preferably 0.3 to 1mm.This can have suitable radius and reach by the basal edge that makes above-mentioned overflow ducts.
Technology of the present invention demonstrate use the N-of moisture tertiary amine oxide particularly the cellulose solution in N-methylmorpholine-N-oxide (NMMO) as the spinning solution advantageous particularly.
The present invention will further do to explain in detail with following examples with reference to the accompanying drawings.
This figure schematically describes spinning plate 1, spinning solution 2 is spun thus to gas phase media for example in the surrounding air, spinning solution is immersed in the solidification liquid that flows downward then, and remain in this solidification liquid until inflexion point 4, behind this point, the silk 5 sudden change ground deflections of having solidified are simultaneously reeled this silk with coiler device 6 then to coiler device 6, for example be wound on the bobbin that is positioned on the coiler device, bobbin is not drawn in addition.During the sudden change deflection of inflexion point 4, most solidification liquid continues to flow downward (seeing the liquid stream 10 that has arrow), thereby removes most of solidification liquid from silk 5 at least.This moment is if to pull out tow be favourable with 45 to 60 degree angles, and angle refers to the angle of 5 of liquid stream 10 and silks.
Storage tank 8 is used to store solidification liquid 7, and quantitative solidification liquid is not had in the turbulent flow ground input storage tank as far as possible, and employed instrument shows.In order to obtain the liquid stream of the solidification liquid 7/3 of stratified flow as far as possible at immersion point place, the storage tank 8 of solidification liquid 7 is by the overflow ducts 9 restriction liquid streams in spinning solution 2 directions, from here by solidification liquid 7 is dosed in the storage tank 8 continuously and consistently, obtain the solidification liquid stream of certain depth, liquid flow to few stratified flow shape basically, and flows to spinning solution 2.Thereby liquid level and the curve of overflow ducts 9 difference in height that transfer vertical direction place of the immersion of spinning solution 2 point place solidification liquid speed by solidification liquid 7 in the storage tank 8 determined.As aforementioned, solidification liquid calculates at the square root of the speed that immerses point by the product of two times acceleration of gravity and difference in height h.
Below will be further in detail with reference to comparative example and embodiment of the invention explanation the present invention.
Embodiment
The spinning solution of Shi Yonging all contains 15% cellulose, 10% water and 75% NMMO in all embodiments; The NMMO spinning solution originates from chemical wood pulp V65 and can obtain from Buckeye, uses the known technology of preparation NMMO spinning solution.With keeping temperature is spinning solution spinning in air of 120 ℃.The aperture of used spinning plate is 200 μ m, squeezes out mass flow m by spinning plate thus.After the gas zone of 18cm, spinning solution enters coagulating bath, and is pulled to coiler device in the terminal of bathing to become 60 degree angles with spinning solution actual flow direction.Coiler device is reeled silk with silk speed Vsp, can not rupture when selecting silk speed to make undrawn yarn.Vsp is the maximum winding speed that does not rupture when making silk.(comparative example) uses fixing coagulating bath (coagulating bath liquid is Ue=0m/min in the speed that immerses point) in embodiment 1-3, and the device of in embodiment 4-6, describing among the use figure, to enter the speed Ue at the immersion point place of solidification liquid be main to spinning solution in this process.Further process data and result have been summed up in the following tabulation.
Table
Embodiment 12345678
m g/h 27.5 34.2 49.1 88.4 35.3 37.0 43.2 57.6
u E m/min 0 0 0 0 60 60 60 60
v sp?m/min 850 950 990 850 1210 1200 1200 1200
Fiber number dtex 0.81 0.9 1.24 2.6 0.73 0.77 0.9 1.2
If use technology of the present invention rather than common fixedly coagulating bath, embodiment has shown can use obviously high winding speed.

Claims (12)

1. make the technology of cellulose fibre, the spinning of cellulose solution that contains dissolving by extruding enters in the gas phase media through a predetermined gas zone, immerse through a predetermined solidification zone then and guiding by coagulating bath, the traction gained cellulose fibre and with its coiling, it is characterized by after gas zone, the spinning solution of extruding is immersed one to be accelerated in the solidification liquid of predetermined speed, and solidification liquid at least near the direction of the spinning solution that squeezes out with Laminar Flow, the solidification liquid side direction enters in the approach of spinning solution thus, and the flow direction of spinning solution and solidification liquid is at whole solidification zone keeping parallelism at least roughly, and lateral deflection when the gained cellulose fibre leaves solidification zone, reel then.
2. according to the technology of claim 1, it is characterized by the solidification liquid that enters spinning solution from a side and have 1.0 to 5mm the constant flow of liquid degree of depth.
3. according to the technology of claim 2, it is characterized by liquid flow depth degree is adjusted to 1-3 times that is about the spinning solution maximum gauge of extruding.
4. according to one or the multinomial technology of claim 1-3, the solidification liquid speed that it is characterized by at spinning solution immersion point place is adjusted to 30-200m/min.
5. according to the technology of claim 4, the speed that it is characterized by solidification liquid is adjusted to 50-80m/min.
6. according to one or the multinomial technology of claim 1-5, the length adjustment that it is characterized by solidification zone is 0.5-8cm.
7. according to the technology of claim 6, the length adjustment that it is characterized by solidification zone is 1-4cm.
8. according to one or the multinomial technology of claim 1-7, it is characterized by the cellulose fibre that solidifies and after solidification zone, become the angular deflection of 45-60 degree with flow direction for solidification liquid.
9. according to one or the multinomial technology of claim 1-8, the cellulose fibre that it is characterized by gained after solidification zone from the flow direction sudden change ground deflection of solidification liquid.
10. according to one or the multinomial technology of claim 1-9, it is characterized by the flow direction deflection of the cellulose fibre sudden change ground of gained after solidification zone from solidification liquid, the radius of its deflecting region is 0.2-2mm.
11., it is characterized by radius and be adjusted to 0.3-1mm according to the technology of claim 10.
12. according to one or the multinomial technology of claim 1-11, it is characterized by with the N-of moisture tertiary amine oxide particularly the cellulose solution in N-methylmorpholine-N-oxide (NMMO) as spinning solution.
CN 96192977 1995-03-31 1996-03-19 Method of producing cellulose fibres Pending CN1180385A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 96192977 CN1180385A (en) 1995-03-31 1996-03-19 Method of producing cellulose fibres

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19512053.1 1995-03-31
CN 96192977 CN1180385A (en) 1995-03-31 1996-03-19 Method of producing cellulose fibres

Publications (1)

Publication Number Publication Date
CN1180385A true CN1180385A (en) 1998-04-29

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CN 96192977 Pending CN1180385A (en) 1995-03-31 1996-03-19 Method of producing cellulose fibres

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CN (1) CN1180385A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1329564C (en) * 2002-05-24 2007-08-01 齐默尔股份公司 Wetting unit and spinning equipment with wetting unit
CN110872732A (en) * 2018-08-30 2020-03-10 奥若泰克股份有限公司 Method and device for spinning filaments by deflection
CN111155183A (en) * 2019-12-31 2020-05-15 中国纺织科学研究院有限公司 Continuous preparation method of cellulose fiber
CN114575040A (en) * 2022-02-24 2022-06-03 北京林业大学 Cellulose spray cloth and preparation method and application thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1329564C (en) * 2002-05-24 2007-08-01 齐默尔股份公司 Wetting unit and spinning equipment with wetting unit
CN110872732A (en) * 2018-08-30 2020-03-10 奥若泰克股份有限公司 Method and device for spinning filaments by deflection
CN110872732B (en) * 2018-08-30 2022-02-15 奥若泰克股份有限公司 Method and device for spinning filaments by deflection
CN111155183A (en) * 2019-12-31 2020-05-15 中国纺织科学研究院有限公司 Continuous preparation method of cellulose fiber
CN111155183B (en) * 2019-12-31 2021-08-31 中国纺织科学研究院有限公司 Continuous preparation method of cellulose fiber
CN114575040A (en) * 2022-02-24 2022-06-03 北京林业大学 Cellulose spray cloth and preparation method and application thereof

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