CN110578179A - Production method and production device of cellulose fiber filaments - Google Patents
Production method and production device of cellulose fiber filaments Download PDFInfo
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- CN110578179A CN110578179A CN201810587593.4A CN201810587593A CN110578179A CN 110578179 A CN110578179 A CN 110578179A CN 201810587593 A CN201810587593 A CN 201810587593A CN 110578179 A CN110578179 A CN 110578179A
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- cellulose
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- liquid
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- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title description 44
- 239000007788 liquid Substances 0.000 claims abstract description 89
- 229920002678 cellulose Polymers 0.000 claims abstract description 64
- 239000001913 cellulose Substances 0.000 claims abstract description 64
- 238000000034 method Methods 0.000 claims abstract description 62
- 239000000835 fiber Substances 0.000 claims abstract description 22
- 238000007711 solidification Methods 0.000 claims abstract description 19
- 230000008023 solidification Effects 0.000 claims abstract description 18
- 238000004140 cleaning Methods 0.000 claims description 64
- 230000015271 coagulation Effects 0.000 claims description 58
- 238000005345 coagulation Methods 0.000 claims description 58
- LFTLOKWAGJYHHR-UHFFFAOYSA-N N-methylmorpholine N-oxide Chemical compound CN1(=O)CCOCC1 LFTLOKWAGJYHHR-UHFFFAOYSA-N 0.000 claims description 48
- 239000000243 solution Substances 0.000 claims description 46
- 239000002904 solvent Substances 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 26
- 230000001112 coagulating effect Effects 0.000 claims description 19
- 238000005507 spraying Methods 0.000 claims description 16
- 238000004804 winding Methods 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 11
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- WFPZPJSADLPSON-UHFFFAOYSA-N dinitrogen tetraoxide Chemical compound [O-][N+](=O)[N+]([O-])=O WFPZPJSADLPSON-UHFFFAOYSA-N 0.000 claims description 9
- 238000007380 fibre production Methods 0.000 claims description 9
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 7
- 239000002608 ionic liquid Substances 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 3
- 229920006324 polyoxymethylene Polymers 0.000 claims description 3
- -1 polyoxymethylene Polymers 0.000 claims description 2
- 238000009987 spinning Methods 0.000 description 28
- 238000000746 purification Methods 0.000 description 9
- 238000011084 recovery Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- FHDQNOXQSTVAIC-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCN1C=C[N+](C)=C1 FHDQNOXQSTVAIC-UHFFFAOYSA-M 0.000 description 2
- QVRCRKLLQYOIKY-UHFFFAOYSA-M 1-methyl-3-prop-2-enylimidazol-1-ium;chloride Chemical compound [Cl-].C[N+]=1C=CN(CC=C)C=1 QVRCRKLLQYOIKY-UHFFFAOYSA-M 0.000 description 2
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 description 2
- 239000005750 Copper hydroxide Substances 0.000 description 2
- 229920000297 Rayon Polymers 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910001956 copper hydroxide Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- IVNPXOUPZCTJAK-UHFFFAOYSA-N 4-methylmorpholin-4-ium;hydroxide Chemical compound O.CN1CCOCC1 IVNPXOUPZCTJAK-UHFFFAOYSA-N 0.000 description 1
- 241000981770 Buddleja asiatica Species 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 229920000875 Dissolving pulp Polymers 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- JXLHNMVSKXFWAO-UHFFFAOYSA-N azane;7-fluoro-2,1,3-benzoxadiazole-4-sulfonic acid Chemical compound N.OS(=O)(=O)C1=CC=C(F)C2=NON=C12 JXLHNMVSKXFWAO-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- QKSIFUGZHOUETI-UHFFFAOYSA-N copper;azane Chemical compound N.N.N.N.[Cu+2] QKSIFUGZHOUETI-UHFFFAOYSA-N 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- RAYLUPYCGGKXQO-UHFFFAOYSA-N n,n-dimethylacetamide;hydrate Chemical compound O.CN(C)C(C)=O RAYLUPYCGGKXQO-UHFFFAOYSA-N 0.000 description 1
- WHQSYGRFZMUQGQ-UHFFFAOYSA-N n,n-dimethylformamide;hydrate Chemical compound O.CN(C)C=O WHQSYGRFZMUQGQ-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D13/00—Complete machines for producing artificial threads
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D4/00—Spinnerette packs; Cleaning thereof
- D01D4/02—Spinnerettes
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
- D01F2/10—Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either
Abstract
The present application relates to a process for producing cellulose fiber filaments using a cellulose solution, comprising: 1) metering and pressurizing a cellulose solution and passing the solution through a spinneret comprising a plurality of capillary openings to form a plurality of solution streams; 2) enabling the solution flow to pass through the first air layer and enter the heat exchange layer; 3) a transversely flowing temperature-controlled air flow is arranged in the heat exchange layer, and the transversely flowing temperature-controlled air flow and the solution flow exchange heat; 4) the heat-exchanged solution flows through the air layer II and then forms fibers through the reversing device, and the reversing device is arranged to be opposite to the liquid in the solidification liquid collecting tank, and the position of the reversing device can be changed between the condition that the reversing device is partially immersed in the solidification liquid and the condition that the reversing device is not contacted with the liquid in the solidification liquid collecting tank. The application also relates to an apparatus for producing cellulose fiber filaments using the cellulose solution.
Description
Technical Field
The invention relates to the field of cellulose fibers, in particular to a production method and a production device of cellulose fiber filaments.
Background
In the field of cellulose fiber production, two main processes are known so far. The first one is a viscose process in which natural cellulose such as wood pulp, cotton pulp, etc. is treated with an alkali solution, the alkali solution is recovered, the remaining part is pulverized, aged, and used with CS2Dissolving the cellulose sulfonate after yellowing into alkali liquor, curing, filtering, defoaming, extruding into a coagulating bath containing sulfuric acid or sulfate through a neck mold,the cellulose sulfonate is regenerated again to cellulose in the gel state in the acid bath. During the regeneration of cellulose sulphonate to cellulose, sulphur-containing products, such as H, are liberated2S、CS2And the like. The process has a large amount of reserves in the market at present, but the national policy has limited the development of the items due to serious environmental pollution, high energy consumption and product quality.
The cuprammonium process is another method of making cellulose fibers. Copper sulfate reacts with ammonium hydroxide to generate copper hydroxide precipitate, sulfate is washed away, and then the copper hydroxide is dissolved in concentrated ammonia water to generate complex tetrammine hydroxide, and the copper-ammonia complex solvent is also one of the earliest solvents of cellulose, and has a plurality of defects: 1) the process is complex and the production efficiency is low; 2) the recovery cost of chemical substances such as ammonia water, sulfate and the like is high; 3) a large amount of salt byproducts such as sodium sulfate, ammonium sulfate and the like can be generated in the production process; 4) by adopting the process, the processing performance of the modified cellulose, the cellulose derivative or the blended cellulose and the synthetic polymer is not ideal;
Due to the above-mentioned disadvantages of the viscose process and the cuprammonium process, many researchers have been working on the research of new solvents for cellulose to find new processes for the production of cellulose products. Representative of these cellulosic solvent systems are: n, N-Dimethylacetamide (DMAC)/lithium chloride (LiCl), N-Dimethylformamide (DMF)/dinitrogen tetroxide (N2O4) Dimethyl sulfoxide (DMSO)/polyoxymethylene ((CH)2O)X) N-methylmorpholine-N-oxide (NMMO)/water, ionic liquids, and the like, and these solvent systems are mixed with cellulose to prepare a uniform cellulose solution, which is then extruded from the capillary holes of a spinneret into an air layer, and then completely immersed in a coagulation bath in which the cellulose is coagulated and formed to form cellulose fibers. The key of the process is to select a proper solvent or ionic liquid, and although some solvents or ionic liquids can well dissolve cellulose, the problems of environmental pollution, difficult solvent recovery and purification and high cost also exist. The solvent selected by the project for realizing the industrial production at present is a solvent system consisting of nontoxic and pollution-free N-methylmorpholine-N-oxide (NMMO), NMMO and waterThe method can well dissolve cellulose, has no chemical reaction in the whole process, has high NMMO recovery efficiency, avoids the problem of serious pollution in the traditional process, and is called as a green process. The cellulose solution prepared by using NMMO as a solvent is generally subjected to dry-jet wet spinning during spinning. Patent CN94192192.1 describes a process for producing cellulose filaments from a cellulose solution: as shown in fig. 1, the solution is first extruded through a spinneret 1a having a plurality of orifices to form a plurality of streams of fiber solution 2a, which are then passed transversely through an air gap 3a into an aqueous spin bath 4a to form cellulosic fiber filaments 11 a. In this process, the fibers need to enter an aqueous spin bath where the cellulose is formed into filaments.
Patent CN0286064.3 describes a spinning apparatus and method for producing a continuous shaped body from a shaped material, wherein the shaped material is extruded through an extrusion orifice into a substantially filament-shaped continuous shaped body, which is then passed successively through a shielding zone, a cooling zone and into a coagulation bath to form the continuous shaped body. In this process, the continuous shaped body must also be passed into a coagulation bath in which the cellulose is formed into a continuous shaped body.
At present, the process for producing cellulose fiber by using NMMO basically needs a coagulating bath, and the cellulose can be rapidly coagulated and formed into fiber only if a solution flow is completely immersed into the coagulating bath. However, the freshly formed filament bundle is subjected to a great resistance by the coagulation liquid during its passage through the coagulation bath, which causes an unnecessary drawing of the filament bundle. The higher the spinning speed is, the resistance is multiplied, and the drafting caused to the tows is also increased; once the drawing of the tow causes the tow to break, production has to be stopped. In order to reduce the resistance drafting of the tows as much as possible in the current industrial project, the spinning speed can only be controlled to be about 40 m/min, so that the spinning efficiency is very low, the equipment is dispersed, and the occupied area is too large.
Disclosure of Invention
Embodiments of the present application provide a method and apparatus for producing cellulose fiber filaments using a cellulose solution.
In a first aspect, embodiments herein provide a method of producing cellulose fiber filaments using a cellulose solution, which may include:
1) Metering and pressurizing a cellulose solution and passing the solution through a spinneret comprising a plurality of capillary openings to form a plurality of solution streams;
2) Enabling the solution flow to pass through the first air layer and enter the heat exchange layer;
3) A transversely flowing temperature-controlled air flow is arranged in the heat exchange layer, and the transversely flowing temperature-controlled air flow and the solution flow exchange heat;
4) And the solution flow after heat exchange passes through the air layer II and then forms fibers through the reversing device, the reversing device is arranged to be capable of changing the relative position with the liquid in the solidification liquid collecting tank between the state that the reversing device is partially immersed in the solidification liquid and the state that the reversing device is not contacted with the liquid in the solidification liquid collecting tank, and the solidification liquid collecting tank is used for containing the solidification liquid.
In one embodiment, the reversing device is arranged without contact with the liquid in the coagulation liquid collecting tank, and a coagulation liquid spraying device is arranged around the reversing device.
In yet another embodiment, the reversing device may be a speed-controllable wire guide device.
In another embodiment, the method may further comprise cleaning the fibers guided out by the reversing device through at least one cleaning roller set, wherein the cleaning roller set may be composed of a pair of cleaning rollers arranged in a non-parallel manner, and a cleaning liquid spraying device may be arranged around the cleaning roller set. Preferably, the cleaning rollers have a non-zero included angle between their respective roller axes, preferably 0.1 ° to 5 °.
In yet another embodiment, the method can further comprise drying the washed fiber through at least one set of drying rolls, wherein the set of drying rolls can consist of a pair of drying rolls arranged in a non-parallel arrangement.
In yet another embodiment, the method may further comprise winding the dried fiber through at least one winder, wherein the winder may employ tension control during the winding process.
In yet another embodiment, the fibers may be individually helically wound in bundles of cellulose filament tows through a set of wash rolls and a set of dryer rolls, respectively.
In yet another embodiment, the solvent portion of the cellulose solution may be selected from the group consisting of a mixture of water and N-methylmorpholine-N-oxide (NMMO), a mixture of DMAC and LiCl, DMF and N2O4Mixture of (A), (B), (C), (D), (E2O)XA mixture of (polyoxymethylene), a specific ionic liquid such as any one of 1-allyl-3-methylimidazolium chloride, 1-butyl-3-methylimidazolium chloride, and the like. The coagulating or cleaning liquid may consist of water and the solvent portion of the cellulose solution. Preferably, the solvent part or the coagulating liquid of the cellulose solution may be an aqueous solution of NMMO with a mass content of 1% to 30%, and the cleaning liquid may be an aqueous solution of NMMO with a mass content of 0% to 30%.
In a second aspect, the present invention provides an apparatus for producing cellulose fiber filaments by the method of the first aspect, which may sequentially include a spinneret, an air gap, a reversing device, a coagulation liquid collecting tank, at least one set of washing roller set, at least one set of drying roller set, and at least one winding device according to a fiber production process, wherein the air gap may include two air layers and a heat exchange layer sandwiched therebetween.
In one embodiment, the spinneret may comprise a plurality of capillary hole groups, each capillary hole group may comprise at least one capillary hole, each capillary hole group may have the same number of capillary holes, and the spacing between two adjacent capillary hole groups is larger than the spacing between two adjacent individual capillary holes, preferably larger than 10 mm.
In another embodiment, a bundling device can be arranged between the reversing device and the cleaning roller group.
In yet another embodiment, the drying roller may be heated using electric energy or a heat medium.
In a further embodiment, a diverting member may be arranged between the set of drying rolls and the windup. The steering member may be a speed-controlled godet roller, a godet hook, a godet wheel, or a non-rotatable godet bar.
Drawings
FIG. 1 is a schematic representation of a prior art cellulose fiber production process.
FIG. 2 is a schematic view of the cellulose fiber filament production process of the present invention, wherein FIG. 2A shows the case where the inverting device is not in contact with the liquid in the coagulation liquid collection tank, and FIG. 2B shows the case where the inverting device is partially immersed in the coagulation liquid.
Fig. 3 is a schematic structural view of a cellulose fiber filament production apparatus of the present invention.
fig. 4 is a top view of the production apparatus of fig. 3.
Fig. 5 is a schematic diagram of a cleaning method in the prior art.
Fig. 6 is a schematic view of another cleaning method of the prior art.
The reference numerals are explained below:
1 a-a spinneret plate; 2 a-a cellulose solution stream; 3 a-air gap; 4 a-a spinning slot; 5 a-gas forced to flow in the air gap; 11 a-cellulose fibres
1-spinneret plate; 2-a flow of cellulose solution; 3-air layer one; 4-heat exchange layer; 5-air layer two; 6-a reversing device; 7-a solidification liquid spraying device; 8-solidification liquid; 9-a solidification liquid collecting tank; 10-a temperature controlled air flow; 11-cellulose filaments; 12-a bundling means; 13-a cleaning solution spraying device; 14-a first set of cleaning rollers; 14U-cleaning roller I; 14D-cleaning roller II; 15-a second set of cleaning rollers; 15U-cleaning roller I; 15D-cleaning roller II; 16-drying roller group; 16U-drying roller I; 16D-a second drying roller; 17-a reversing component; 18-a winding device; 19 a-a bundle of bundled filaments; 19 b-cellulose filaments after the first washing; 19 c-cellulose filaments after the second washing; 19 d-dried cellulose filaments; 20-cleaning the tows; 21-cleaning a water curtain; 22-cleaning bath.
Detailed Description
As mentioned above, in the prior art cellulose fiber production methods, cellulose is coagulated and formed by passing a cellulose solution stream through a spinning tank or a coagulation bath, and for this reason, the spinning speed has to be controlled to about 40 m/min. The method is not only suitable for the production of short fibers which are subjected to a large amount of spinning by a spinneret plate each time and are subjected to subsequent cutting and the like, but also can not meet the production requirements of cellulose fiber filaments at all, because the number of the filaments which are spun by the spinneret plate each time in the filament production is limited, the quality requirements of the filaments are very strict due to the subsequent direct application of the produced filaments, and the whole production has to be stopped due to the breakage of a single filament in the production.
In the process according to the invention for producing cellulose fibre filaments from a cellulose solution, the travel of the cellulose coagulated in the coagulation bath out of the coagulation bath is significantly reduced, even completely without coagulation in the coagulation bath, but instead the coagulation is carried out on a deflecting device, on the surface of which a coagulation liquid is sprayed, whereby the resistance to the freshly formed tow during its passage through the coagulation bath is significantly reduced or virtually completely eliminated, which is particularly advantageous for the production of cellulose fibre filaments of the desired fibre quality at the desired production rate.
Specifically, as shown in fig. 2, in the method of producing cellulose fiber filaments according to the present invention, a cellulose solution is first metered and pressurized and then passed through a spinneret 1 including a plurality of capillary holes to form a plurality of solution streams 2.
The cellulose solution is a homogeneous liquid formed by completely dissolving cellulose in a solvent, wherein the solvent may be a mixture of water and NMMO (abbreviated as "H2O/NMMO "), mixtures of DMAC and LiCl (DMAC/LiCl), DMF and N2O4Mixture of (DMF/N)2O4) DMSO and (CH)2O)XThe mixture of (a), a specific ionic liquid such as 1-allyl-3-methylimidazolium chloride salt, 1-butyl-3-methylimidazolium chloride salt, and the like. Preferably, the solvent is H2O/NMMO. The mass content of the cellulose in the cellulose solution can be 4-18%.
The spinneret 1 may comprise a plurality of capillary hole groups, each of which may comprise at least one capillary hole, and each of which may have the same number of capillary holes. For example, the spinneret plate 1 may include 6 capillary hole groups (as shown in fig. 4), each capillary hole group has 20 to 1000 capillary holes, the distance between adjacent capillary hole groups is 10 to 30 mm, and the distance between individual capillary holes is 1 to 5 mm. The specific number of capillary openings depends on the type and size of the fibers. The diameter of the capillary openings can be 0.08 to 0.3 mm, depending on the thickness of the filaments to be produced. The spacing between two adjacent groups of capillary openings can be significantly greater than the spacing between two adjacent individual capillary openings, preferably greater than 10 mm, which facilitates the necessary manual handling and allows the filaments to which each monofilament belongs to be readily identified.
After passing through the air layer one 3, the solution flow 2 enters the heat exchange layer 4. The height of the air layer I3 can be 5-200 mm, and the height of the heat exchange layer 4 can be 10-100 mm. The temperature-controlled air flow transversely flows in the heat exchange layer 4, wherein the temperature of the air flow can be 5-40 ℃, and the relative humidity can be not more than 90%. In the heat exchange layer 4, the temperature of the cellulose solution flow 2 is controlled, a small amount of cellulose exists, the surface viscosity is reduced, and the fiber forming is facilitated. The temperature of the solution flow 2 is controlled in the heat exchange layer 4 and then reaches the reversing device 6 through the air layer II 5.
The reversing device 6 can be a speed-controllable thread guide device, and a solidification liquid collecting tank 9 is used for containing solidification liquid 8. In fig. 2A, the direction changing device 6 is arranged without contact with the liquid in the coagulation liquid collecting tank 9, and a device 7 for spraying the coagulation liquid is arranged around it, and the spraying device 7 can quantitatively spray the coagulation liquid 8 to the direction changing device 6 or the solution flow 2.
The coagulating liquid 8 is composed of water and a solvent in a cellulose solution, and may be, for example, water and DMAC/LiCl, water and DMF/N2O4Water and DMSO/(CH)2O)XWater and NMMO, or water and an ionic liquid. Preferably, the solidification liquid 8 consists of water and NMMO, wherein the mass content of NMMO is 1% -30%. The solution flow 2 is under the action of the coagulating liquid 8, the cellulose therein is formed into fibers 11, and the solvent part is carried by the coagulating liquid 8 to the coagulating liquid collecting tank 9.
In the method of the invention, the reversing device 6 may be arranged such that its position relative to the liquid in the coagulation liquid collection tank 9 may be varied between partial immersion of the reversing device in the coagulation liquid and no contact with the liquid in the coagulation liquid collection tank. As shown in fig. 1, in the prior art, the reversing device (such as a godet) is usually completely immersed in the coagulation bath, which makes the travel path of the cellulose in the coagulation bath out of the coagulation bath very long, and thus the resistance to the cellulose is also large. According to the invention, as shown in fig. 2B, the reversing device can be only partially immersed in the coagulating liquid, which can be conveniently achieved by draining off some of the coagulating liquid or adding little coagulating liquid in advance, for example, only 15% of the reversing device is immersed in the coagulating liquid. Therefore, the traveling path of the cellulose in the coagulating liquid passing out of the coagulating liquid is obviously shortened, and the resistance suffered by the fiber filaments in the process of passing out of the coagulating liquid is obviously reduced.
The reversing device 6 can be a speed-controlled thread guide device, for example a godet roller. When the reversing device is partially immersed in the solidified liquid, the reversing device 6 can not rotate (for example, can be used as a driven roller of a subsequent cleaning roller), and the speed is 0, so that the liquid level fluctuation and even splashing are avoided, and the resistance suffered by the fiber filaments in the process of penetrating out of the solidified liquid is further increased. When the reversing device is arranged without contact with the liquid in the coagulation liquid collection tank, the reversing device 6 is preferably rotated, which can greatly increase the spinning speed. The rotating speed of the reversing device can be determined according to the spinning speed and the diameter of the reversing device. For example, the spinning speed can be 40-280 m/min, a guide wire device with a diameter of 150 mm is selected, and the rotating speed can be 85-595 r/min correspondingly.
figures 3 and 4 show a complete schematic representation of a cellulose fibre filament production plant according to the invention. The subsequent steps of the process for the production of cellulose fiber filaments according to the invention will be further described with reference to fig. 3 and 4.
As shown in FIG. 3, the fibers 11 are composed of a large number of monofilaments having a fineness of 1.1 to 3.3Dtex, and are bundled by a bundling device 12 into a filament bundle 19a having a constant fineness. As can be seen from fig. 4, 6 filament bundles were bundled together. The bundling means 12 is typically made of a ceramic piece, which may be in the shape of a U, a dog tail, etc.
Filament bundle 19a contains a large amount of solvent and must be cleaned. The filament bundle 19a is cleaned by the cleaning roller group 14. The cleaning roller group 14 is constituted by a pair of cleaning rollers 14U, 14D arranged in non-parallel. The pair of washing rollers can be arranged up and down, or can be arranged horizontally or obliquely, preferably up and down, because the whole device can be made compact. The diameters of the two cleaning rollers may be the same or different, but the respective roller axes should have a certain included angle, for example, 0.1 ° to 5 °, between them to ensure that the filament bundles 19a do not overlap when spirally winding on the cleaning roller group 14, thereby extending the winding length of the filament bundles 19a on the cleaning roller group 14 and ensuring the cleaning cleanness. The pitch of the spiral of the filament bundle 19a on the cleaning roller group 14 depends on the diameter of the cleaning rollers and the angle between the axes of the two cleaning rollers. As shown in fig. 3 or 4, the two cleaning rollers 14U and 14D are arranged vertically, the upper roller 14U is vertical, the lower roller 14D is inclined horizontally to the right by an angle α, and the diameter of the lower roller 14D is D, so that the thread pitch D of the filament bundle 19a passing over the cleaning roller group 14 is D tan (α).
The washer fluid spray device 13 may be arranged around the washer roller group 14 to spray washer fluid to the washer roller group 14 and/or the filament bundle 19 a. The cleaning liquid may be composed of water and a solvent in the cellulose solution, and the mass content of water is preferably 70% to 100%, more preferably 95% to 100%.
According to the residual index requirement of the solvent in the filament bundle, a plurality of groups of cleaning roller sets can be arranged. As shown in fig. 3 or 4, two sets of cleaning roller sets 14, 15 are provided, and the water content of the cleaning liquid used in each set of cleaning roller sets is preferably different, so that the cleaning effect can be ensured and the cost of solvent purification can be reduced.
Compared with the traditional cleaning mode, the cleaning mode has the advantages that the structure is compact, the occupied area is small, and in the process adjustment, the cleaning time of the tows can be changed by simply adjusting the number of the winding turns of the tows in the cleaning roller set, so that the cleaning effect is achieved. Fig. 5 and 6 show two cleaning methods in the prior art. FIG. 5 is a cleaning method by adopting a multi-roller combination and a cleaning water curtain, and FIG. 6 is a cleaning method by completely immersing the tows in the cleaning liquid, wherein the two methods have the defects of large equipment investment, large floor area and difficult process adjustment once the equipment is shaped.
After the filament bundle 19a is cleaned, the residual index of the solvent has reached the requirement, generally not more than 500ppm, but the water content is still high, so that drying is required. As shown in fig. 3 or 4, the drying roller set 16 is composed of a pair of drying rollers 16U, 16D arranged in a non-parallel manner, and the arrangement method of the pair of drying rollers and the included angle between the roller axes are the same as those of the cleaning roller set, and the winding distance and the winding length of the filament tows on the drying roller set need to be ensured, so that the drying effect of the filament tows is ensured. In general, it is necessary to ensure that the final moisture content of the dried filament bundle 19d is not higher than 10 mass%. The drying rollers 16U, 16D may be heated by electric energy or by a heat medium. Preferably, hot water can be used as the heat medium, so that not only energy costs are low, but also manufacturing costs of the apparatus can be reduced.
The dried filament bundle 19d is wound into a cake of a predetermined weight by a winding-up device 18. The winding and winding device 18 may be a plurality of winding devices or one winding device. Tension control may be employed throughout the wrapping process.
Between the winding-up device 18 and the drying roller set 16, a deflecting element 17 can be provided to change the direction of travel of the filament bundle 19d in order to better cooperate with the winding-up device 18. The diverting member 17 may be a godet, godet wheel, godet roll or godet bar, etc. Preferably, godet rolls are used with a controlled speed, so that the tension of the filament bundle can be adjusted.
the method for producing the cellulose fiber filament can improve the spinning speed by 4-7 times compared with the prior art on the basis of ensuring the reliability, and can reach 160-280 m/min, thereby obviously improving the production efficiency and reducing the equipment investment.
Hitherto, as NMMO/H2The industrial production of cellulose fibres in solvent O is almost entirely focused on short fibre production and the thread guide needs to be completely immersed in the coagulation liquid to make the cellulose, resulting in spinning speeds of up to 40 m/min. Because if the spinning speed reaches 50 m/min or more, the friction between the fibers and the coagulation liquid brings a large amount of the coagulation liquid to make the coagulation liquid level fluctuate like a boiling state. This problem has long existed, but no one has so far attempted to solve it, but rather has been better toleratedLow spinning speed and unnecessary drawing of the filaments. This is not so demanding as to quality, and it is industrially acceptable for the as-formed tow to undergo unnecessary drawing due to the resistance experienced during its passage through the coagulation bath, and staple fiber production is not yet acceptable, but it is not at all feasible for the production of cellulose fiber filaments of the required fiber quality and the required yield. Therefore, the technical scheme of the invention solves the technical obstacles always puzzling the technical personnel in the field and brings about the leap of the spinning speed and the spinning efficiency.
On the other hand, the process of the invention is obviously equally applicable to the production of staple fibres. It is within the contemplation of the invention to remove the guide wire apparatus step by step from complete immersion in the coagulation liquid (or to reduce the coagulation liquid step by step) prior to fiber production.
The invention also provides a device for producing the cellulose fiber filaments. As shown in fig. 3 and 4, the apparatus may include a spinneret 1, an air gap, a reversing device 6, a coagulation liquid collecting tank 9, at least one washing roller set 14, at least one drying roller set 16, and at least one winding device 18 in this order according to a fiber production process, and the air gap may include two air layers and a heat exchange layer sandwiched therebetween. The above description of the apparatus or equipment in the production method of the present invention is applicable to the apparatus for producing cellulose fiber filaments of the present invention.
Examples
The invention is illustrated in more detail below by way of examples, for a total of 9 examples, including comparative examples 1-3 and examples 4-9. The operating conditions of the examples are specified in table 1, wherein all contents represent mass contents; the continuous stable production reliability is defined as: one spinneret replacement cycle is 15 days, and the number of times of failures such as broken ends, winding rollers and the like in the period is n, the reliability is (100-n) ÷ 100); the economics of solvent NMMO recovery and purification are measured as the water content of the solvent recovered from the coagulation liquid collection tank, with lower water contents providing better economics of recovery and purification.
Comparative examples 1-3 cellulose filaments were produced using a prior art process, the specifications being: 160Dtex/80f, single filament fineness 2 Dtex. The depth of the coagulation bath was 200 mm.
The mass concentration of NMMO in the coagulation bath adopted in the comparative example 2 is about 20%, the spinning speed is set to 40 m/min, the continuous and stable production reliability can reach 97%, and the economy of solvent NMMO recovery and purification is moderate.
Comparative example 3 the spinning speed was increased to 45 m/min and the mass concentration of NMMO in the coagulation bath remained constant, still 20%. As a result, the reliability of continuous stable production is obviously reduced to 78%.
Comparative example 1 on the basis of comparative example 3, the mass content of NMMO in the coagulation bath was adjusted to reduce the content to 10%. As a result, the reliability of continuous and stable production is improved to 82%, but the economical efficiency of solvent NMMO recovery and purification is greatly reduced.
Example 5 on the basis of comparative example 2, the spinning speed was slowly increased by lowering the depth of the coagulation bath to 30 mm. Interestingly, when the speed was increased to 62 m/min, the reliability of continuous stable production still reached 96%; however, when the amount of NMMO in the filament bundle 19a was increased, the reliability of continuous stable production was reduced to 82% in the case of 67 m/min, i.e., the condition of example 6. For this purpose, the residence time of the filament bundle on the first cleaning roller group is increased from 20 seconds to 25 seconds; the quality concentration of NMMO in the cleaning liquid used by the first cleaning roller group is reduced to 3% from 5%, the processes of the second cleaning roller group and the drying roller group are kept unchanged, and the final NMMO residual index and the water content index of the tows can meet the requirements.
Example 4 on the basis of example 5, the mass content of NMMO in the coagulation bath was adjusted to reduce the content to 10%, and the continuous stable production reliability could reach 91%, but the economics of solvent NMMO recovery and purification were greatly reduced.
Example 8 completely eliminated the coagulation bath, and the mass concentration of the coagulation liquid sprayed was still 20% by arranging a coagulation liquid spraying device around the reversing device. The spinning speed was slowly increased. Surprisingly, the reliability of continuous stable production still reaches 95% when the speed is increased to 160 m/min. When the rate is increased to 170 m/min, which is the case of example 9, the reliability of continuous and stable production is reduced to 92%, and the NMMO content in the filament bundle 19a is increased. The retention time of the tows on the first cleaning roller group is adjusted to be increased from 20 seconds to 30 seconds, the mass concentration of NMMO in cleaning liquid used by the first cleaning roller group is reduced from 5% to 2%, the processes of the second cleaning roller group and the drying roller group are kept unchanged, and the final NMMO residual index and the water content index of the tows can still meet the requirements.
Example 7 on the basis of example 5, the mass content of NMMO in the coagulation bath was adjusted to fall to 10%, and the continuous stable production reliability could surprisingly reach 96%, except that the economics of solvent NMMO recovery and purification were not good.
From these 9 examples it can be seen that the depth of the coagulation bath has a great influence on the spinning speed. By reducing the depth of the coagulation bath from 200 mm to 30 mm, the spinning speed can be increased from 40 m/min to 62 m/min. This is sufficient to demonstrate that the resistance of the coagulation bath is large, which seriously affects the increase in spinning speed.
It can be seen from examples 7 to 9 that the spinning speed is increased far beyond the imagination by removing the coagulation bath and instead spraying the coagulation liquid on the reversing device. By adjusting the process settings of the first and second cleaning roller sets, adverse effects caused by the increase of the NMMO content in the filament bundle 19a can be completely eliminated, and the final NMMO content in the product can be controlled within a required range.
For the production of cellulose fiber filaments, the spinning speed is high or low, and the investment per ton of product energy production is directly related. Only when the investment of ton product energy is reduced to a certain degree, the industrialized production of the cellulose fiber filament can become possible, so that the traditional coagulating bath is cancelled, and the method has great significance.
TABLE 1
| Examples of the invention | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 |
| Depth of coagulation bath (mm) | 200 | 200 | 200 | 30 | 30 | 30 | 0 | 0 | 0 |
| NMMO content in coagulation bath (%) | 10 | 20 | 20 | 10 | 20 | 20 | |||
| NMMO content (%) of coagulation liquid spray | Without spraying | Without spraying | without spraying | Without spraying | Without spraying | Without spraying | 10 | 20 | 20 |
| Linear speed of the reversing device (meter/minute) | 0 | 0 | 0 | 0 | 0 | 0 | 170 | 160 | 170 |
| Spinning speed (meter/minute) | 45 | 40 | 45 | 67 | 62 | 67 | 170 | 160 | 170 |
| NMMO content (%) | 42.3 | 52.3 | 52.5 | 45.7 | 54.7 | 55.0 | 46.8 | 55.4 | 55.7 |
| Residence time (seconds) of the filament bundle in the first cleaning roller set | 20 | 20 | 20 | 25 | 25 | 25 | 30 | 30 | 30 |
| NMMO content (%) | 5 | 5 | 5 | 3 | 3 | 3 | 2 | 2 | 2 |
| NMMO content (%) | 4.9 | 4.8 | 5.0 | 3.5 | 3.3 | 3.4 | 2 | 2 | 2 |
| Residence time (seconds) of the filament bundle in the second cleaning roller set | 20 | 20 | 20 | 20 | 20 | 20 | 20 | 20 | 20 |
| NMMO content (%) | 0.05 | 0.05 | 0.05 | 0.05 | 0.05 | 0.05 | 0.05 | 0.05 | 0.05 |
| NMMO content (PPM) in tow 19c | 487 | 495 | 492 | 482 | 492 | 490 | 492 | 496 | 493 |
| Temperature of drying roller set (. degree. C.) | 110 | 110 | 110 | 110 | 110 | 110 | 110 | 110 | 110 |
| Residence time (second) of filament bundle in drying roller set | 20 | 20 | 20 | 20 | 20 | 20 | 20 | 20 | 20 |
| Moisture content (%) of dried tow 19d | 9.2 | 9.3 | 9.2 | 9.3 | 9.2 | 9.2 | 9.3 | 9.3 | 9.2 |
| Number of capillary holes in each capillary hole group | 80 | 80 | 80 | 80 | 80 | 80 | 80 | 80 | 80 |
| Number of capillary hole groups | 6 | 6 | 6 | 6 | 6 | 6 | 6 | 6 | 6 |
| Single filament fineness (Dtex) | 2 | 2 | 2 | 2 | 2 | 2 | 2 | 2 | 2 |
| Height of air layer (millimeter) | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 |
| Height of heat exchange layer (millimeter) | 20 | 20 | 20 | 20 | 20 | 20 | 20 | 20 | 20 |
| Air flow temperature (DEG C) in the heat exchange layer | 30 | 30 | 30 | 30 | 30 | 30 | 30 | 30 | 30 |
| Air flow velocity (meter/minute) in heat exchange layer | 9 | 9 | 9 | 9 | 9 | 9 | 9 | 9 | 9 |
| Relative humidity of air stream (%) | 90 | 90 | 90 | 90 | 90 | 90 | 90 | 90 | 90 |
| Continuous stable production reliability (%) | 82 | 97 | 78 | 91 | 96 | 82 | 96 | 95 | 92 |
| Economics of NMMO purification | Difference (D) | Is moderate | Is moderate | Difference (D) | Is moderate | Is moderate | Difference (D) | Is moderate | Is suitable for |
Claims (10)
1. A method of producing cellulose fiber filaments using a cellulose solution, comprising:
1) Metering and pressurizing a cellulose solution and passing the solution through a spinneret comprising a plurality of capillary openings to form a plurality of solution streams;
2) Enabling the solution flow to pass through the first air layer and enter the heat exchange layer;
3) A transversely flowing temperature-controlled air flow is arranged in the heat exchange layer, and the transversely flowing temperature-controlled air flow and the solution flow exchange heat;
4) And the solution flow after heat exchange passes through the air layer II and then forms fibers through the reversing device, the reversing device is arranged to be capable of changing the relative position with the liquid in the solidification liquid collecting tank between the state that the reversing device is partially immersed in the solidification liquid and the state that the reversing device is not contacted with the liquid in the solidification liquid collecting tank, and the solidification liquid collecting tank is used for containing the solidification liquid.
2. The method according to claim 1, wherein the reversing device is disposed without contacting the liquid in the coagulation liquid collecting tank, and a coagulation liquid spraying device is disposed around the reversing device.
3. A method according to claim 1 or 2, wherein the diverting means is a speed-controllable thread guide.
4. A method according to any one of claims 1 to 3, characterized in that the method further comprises washing the fibres guided out by the deflecting device through at least one set of washing rollers, wherein the set of washing rollers consists of a pair of washing rollers arranged non-parallel.
5. The method of claim 4 further comprising drying the cleaned fiber through at least one set of dryer rolls, wherein the set of dryer rolls comprises a pair of dryer rolls arranged in a non-parallel relationship.
6. A method according to claim 4 or 5, characterized in that the fibres are individually helically wound in bundles of cellulose filament tows through a set of washing rolls and a set of drying rolls, respectively.
7. the process according to any one of claims 1 to 6, characterized in that the solvent fraction of the cellulose solution is selected from any one of a mixture of water and N-methylmorpholine-N-oxide, a mixture of N, N-dimethylacetamide and lithium chloride, a mixture of N, N-dimethylformamide and dinitrogen tetroxide, a mixture of dimethyl sulfoxide and polyoxymethylene, ionic liquids; the coagulating liquid consists of water and a solvent part of cellulose solution; the solvent part or the coagulating liquid of the cellulose solution is preferably an aqueous solution containing 1 to 30 mass percent of N-methylmorpholine-N-oxide.
8. A method according to any one of claims 4 to 7, characterized in that a washing liquid spraying device is arranged around the set of washing rollers, the washing liquid consisting of water and a solvent part of a cellulose solution, preferably an aqueous solution with a mass content of N-methylmorpholine-N-oxide of 0-30%.
9. An apparatus for producing cellulose fiber filaments by the method according to any one of claims 1 to 8, comprising a spinneret, an air gap, a reversing device, a coagulation liquid collecting tank, at least one cleaning roller set, at least one drying roller set and at least one winding device in sequence according to a fiber production process, wherein the air gap comprises two air layers and a heat exchange layer sandwiched therebetween.
10. The apparatus of claim 9, wherein the spinneret comprises a plurality of capillary hole groups, each capillary hole group comprising at least one capillary hole, each capillary hole group having the same number of capillary holes, and wherein the spacing between two adjacent capillary hole groups is greater than the spacing between two adjacent individual capillary holes, preferably greater than 10 mm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021135705A1 (en) * | 2019-12-31 | 2021-07-08 | 中国纺织科学研究院有限公司 | Cellulose fiber continuous preparation method |
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