CN1168159A - Manufacture of extruded articles - Google Patents
Manufacture of extruded articles Download PDFInfo
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- CN1168159A CN1168159A CN96191362A CN96191362A CN1168159A CN 1168159 A CN1168159 A CN 1168159A CN 96191362 A CN96191362 A CN 96191362A CN 96191362 A CN96191362 A CN 96191362A CN 1168159 A CN1168159 A CN 1168159A
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/05—Filamentary, e.g. strands
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/07—Flat, e.g. panels
- B29C48/08—Flat, e.g. panels flexible, e.g. films
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/88—Thermal treatment of the stream of extruded material, e.g. cooling
- B29C48/919—Thermal treatment of the stream of extruded material, e.g. cooling using a bath, e.g. extruding into an open bath to coagulate or cool the material
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
A method of manufacturing extruded articles of lyocell is described wherein a solution of cellulose in a tertiary amine N-oxide is extruded by way of a die (2) through an air-gap (3) then into a coagulating bath (5), air being supplied to and discharged from the air-gap (3), characterised in that the air-gap (3) comprises a first region (9) adjacent the face (2a) of the die (2) and a second region (12) more remote from the face (2a) of the die (2), the moisture content of the air supplied to the first region (9) being maintained at a lower value than the moisture content of the air supplied to the second region (12). The method provides improved spinnability and may provide lyocell filaments with a reduced tendency to fibrillation.
Description
Invention field
The present invention relates to the manufacture method of cellulosics, in the method, will clamp-on in the spinning bath at the cellulose solution in the dissolving N-tertiary amine oxide with shower nozzle.
The known fiber element may be dissolved in some N-tertiary amine oxides (for convenient, also can be described as amine oxide), forms solution or spinning solution, and described solution or stoste can be clamp-oned with shower nozzle and form moulded products such as fiber and film in the spinning bath.Stoste generally contains the water of fraction, and spinning bath is water bath normally.Wash consolidated article then to remove residual amine oxide.This method is an example of solution spinning, and the fiber that so makes can be described as Lyocell fibre or lyocell fiber.The example of suitable amine oxide is N-methylmorpholine-N-oxide (NMMO).Background technology
U.S. Pat-A-4 that its content is incorporated by reference herein, 261,943 have described a kind of like this solution spinning: will extrude at the cellulose solution among the moisture NMMO with spinning head, by for example 5 or the space of 30cm length, form filament, then it is fed water bath, produce the lyocell fiber thus.This patent has also been described after extruding, and is sprayed on filamentary solution spinning in the space with cellulosic non-solvent liquid such as water immediately.Allegedly be filament clinkering tendency together in the space like this in order to reduce ejection.
International patent application W0-A-93/19230 had described before importing spinning bath, for example with cold air stream will be in the space the solution spinning of filament cooling.The temperature of stoste can be 90-110 ℃, and the temperature of cold air can be-5 to+5 ℃, and gap lengths can be 60-145mm.
Disclosure of an invention
The invention provides the method for the extruded product of a kind of lyocell of manufacturing, in the method, to extrude at the cellulose solution in the N-tertiary amine oxide with shower nozzle, by entering behind the space in the spinning bath, supply air to the space and extract out from the space, the method is characterized in that the space comprises with contiguous the 1st zone of the face of shower nozzle with from the face of shower nozzle the 2nd zone far away, the moisture that is conducted to the air in the 1st zone remains below the level of the moisture of the air that is conducted to the 2nd zone.
The lyocell goods of extruding can be the film or the form of filament (not only comprise may being sheared subsequently and forming the fibre bundle of staple fibre, and comprise filament yarn) preferably.When goods are long filament, claim that usually shower nozzle is a spinning head, the title extrusion method is a spin processes.
The length in the space between shower nozzle and the spinning bath is preferably 10-160mm, better is 15-100mm or 20-60mm.Though should be understood that the gas air preferably in the space, also can be other inert gases such as nitrogen or mist.
The length in two zones in space can be identical or different.In one embodiment, the length in the 1st zone is preferably less than the length in the 2nd zone.The length in the 1st zone is preferably 3-10mm, and like this, the 2nd zone occupies the remaining longer part in space.
Cellulose solution (also can be called stoste) is normally extruded downwards by the space.When using such conventional techniques, preferably with air with the horizontal substantially direction of the direct of travel of stoste extrudate by the space be that horizontal direction is conducted to the space and extracts out from the space.Laterally arrange such, for simplicity, the air flow that flows through the space can be called horizontal air-flow.The air speed that is conducted to the space preferably is 1-20m/sec in two zones, better is 2-10m/sec.The speed Ying Gaozhi that it should be understood that air is enough to keep the neither regional together interior stoste extrudate different air conditions on every side in space, but can not high extremely destruction pass through passing through in order of the stoste extrudate there.Generally speaking, higher speed may cause the above-mentioned destruction than the vast sky crack.Air speed in the 1st and the 2nd zone in space can be identical or different.Can record by simple test at any suitable air speed in particular cases.
The method that from two zones one or both discharge air can be an extracting method.The nozzle of available process appropriate design and suction nozzle are conducted to air the space easily and discharge from the space.Should be understood that the 1st and the 2nd zone respectively needs nozzle separately.More than one suction nozzle can be arranged.In preferred embodiment, each nozzle is towards a suction nozzle onesize with it.So the advantage that is provided with is can control more accurately by each regional stoste extrudate ambient air condition of space; Especially more should be like this during less than the length in the 2nd zone when the length in the 1st zone, and this is desirable exactly.
The temperature of air that is conducted to the space for example, between 0-40 ℃, often is 20-30 ℃ generally about environment temperature.The temperature of stoste that is conducted to shower nozzle is usually between about 80-125 ℃, thereby air flow just plays the effect of the extrudate in the cooling space.According to common practice, the speed that extruded product is batched from spinning bath is higher than the rate of extrusion by the stoste of shower nozzle, its coefficient ratio often between 2.5-25, thereby can stretch extrudate, to reach the purpose of improving its engineering properties.It is believed that such stretching almost all occurs in the space.The scope that the extrudate of cooling in the space tends to take place to stretch is limited to and the immediate part of the face of shower nozzle.The speed of batching of extruded product is preferably between the 5-100m/min.
The moisture of air that is conducted to the 2nd zone in space cans be compared to most the big approximately 1-30g water of the moisture/kg air of the air that is conducted to the 1st zone, better big approximately 10-20g water/kg air.The moisture that is conducted to the air in the 1st zone preferably is about 0-20 water/kg air, better is about 0-10g water/kg air, and the moisture that is conducted to the air in the 2nd zone preferably is about 5-30g water/kg air.
The lyocell fiber has fibrillation tendency usually, especially ought be subjected to the mechanical stress in the damp and hot processed process, during as those mechanical stresses of often running in the fabric production process such as washing, bleaching and dyeing.After the fibrillation, long fiber promptly partly separates from fiber surface, makes fiber (and yarn and fabric of containing these fibers) present the brushy outward appearance that can not make the people produce aesthetic feeling.Be surprised to find already, and compared with the fiber of producing with traditional fibre spinning method, the fibrillation of the fiber of producing with method of the present invention is inclined to less.
Known when carrying out the lyocell spinning, the stoste extrudate, for example the monofilament form breaks end in the space sometimes.This type of fault may owing to stability of spinning process lose or spinnability poor.The evidence of spinnability difference is to can be observed fracture of wire or coherent strand in the product of collecting, or under serious situation, take place to interrupt completely in the space or in coagulating bath.Be surprised to find already, and compared with traditional technology, method of the present invention provides better stability of spinning process, especially in long space.Though this effect is difficult to quantitatively, can easily be confirmed by observing.
Cellulosic average degree of polymerization (D.P.) in the stoste generally can be 250-2000, is preferably 500-2000, better is 750-1000.Have found that, when cellulose D.P. is 750-1000, can under condition in a big way, obtain better spinnability.By measuring the weak solution of cellulose in moisture metal/amine complex solvent such as the viscosity of Kocide SD ammonium salt solution, can calculate the cellulosic degree of polymerization (D.P.) easily.After this test method 3 of Miao Shuing is the suitable method based on TAPPI T206.Cellulose D.P. is a yardstick of estimating the anhydroglucose number in the per molecule.Should be understood that the D.P. that records with this method is sticking equal D.P..
The simple declaration of accompanying drawing
The present invention will be described in more detail below in conjunction with accompanying drawing, and this accompanying drawing is to be applicable to schematic representation of apparatus of the present invention.
With reference to accompanying drawing, with gear pump 1 cellulose solution in aqueous amine oxide, said is supplied to spinning head 2. Stoste can for example contain the cellulose of 5-25 % by weight, the NMMO of 70-85 % by weight and the water of 5-15 % by weight, and former liquid temp can be between 80-125 ℃. Stoste is extruded downwards, by the hole in spinning head 2, entered temperature and remain in the space 3 that is lower than former liquid temp, there, stoste is solidified, and forms a branch of ultimate fibre 4. Then, ultimate fibre 4 passes in the moisture spinning bath 5, partly around cylinder 6 by and be exported coagulating bath so as to clean, dry and other common processing operations. The superficial velocity of cylinder 6 is higher than the speed of the stoste that goes out from the orifice flow of spinning head 2, with stretching ultimate fibre 4. Filamentary stretching major part occurs in the space 3.
With the air supplied with for the first time from blowing nozzle 7 be blown into the 1st contiguous zone of spinning head 2 space 3 in, and with suction nozzle 8 it 3 is extracted out from the space, so that the direct of travel of itself and ultimate fibre 4 laterally passes through space 3. Arrange nozzle 7,8 to such an extent that make this operation play the environment temperature in the 1st zone 9 that the face 2a with spinning head 2 is close to and the effect that humidity remains on desired level. The air that similarly will supply with for the second time is from blowing nozzle 10 is blown into space 3 from 2nd zone 12 of spinning head away from, and with suction nozzle 11 extractions. Arrange nozzle 10,11 to such an extent that make this operation play a part the temperature and humidity in the 2nd zone 12 between the 1st zone 9 and spinning bath 5 is remained on desired level. Nozzle 7 and 10 is given prominence to, and crosses the air of whole bundle ultimate fibre 4 with supply. Confession to the water content of the air of blowing nozzle 7 is lower than the water content that supplies to the air of blowing nozzle 10. The temperature of two kinds of air supplying with can be identical or different.
Although accompanying drawing has been described two kinds of air of different nature for the situation to the space, should be understood that also can be with three kinds or more kinds of air of different nature so for not departing from essence of the present invention to the zones of different in space.
The fibrillation tendentiousness of lyocell fiber can be estimated by following test method(s):
Test method 1 (sand is washed test)
The little bundle fiber that will contain 100-200 root monofilament is cut into 5mm length. Then these short fibers are placed the vial of the 20ml that contains the 4g glass microballoon, add 8ml water. With glass bottle stopper jail, shook 20 minutes with 2800 rev/mins with Stewart flask shaking machine.
The taking-up a few fibres also is placed on the microslide. Light micrograph by fibrillating fibre calculates fibrillation value (Cf). Fibriilar total length f on the fiber of measured length L. The fibrillation value is provided by following equation:
C
f＝∑f/L
This operation can be carried out or carry out with the image analysis method by hand. In addition, can set up one group of standard microphoto for comparing. Have found that trained fibre technology technical staff's evaluation result is with to record the result with this method consistent. In practice, owing to be difficult to find a large amount of fibrillation, therefore, can not measure about fibrillation value more than 30. Data are to record at the mid point of the fiber of length 5mm and end. Experience shows that the result of fiber ends and the correlation of fabric property are best, therefore, only get this value herein as Cf(TM1) numerical value.
Test method 2 (refining-dye test method)
Use following method evaluation fibrillation value (F.I.). Fiber samples is lined up the series that original fiber degree is increase gradually. Then the full-length of measuring fiber in each sample is also calculated the number of the fibrillation (fine, soft fur that stretches from fibrous body stings) along full-length. Measure each fibriilar length, and determine by the fibril dimension multiply by fibriilar average length and the arbitrary value of each fiber. The fiber of this arbitrary value maximum is regarded as the fiber of easily fibrillable and its any fibrillation value is decided to be 10. With fully not the fibrillation value of the fiber of fibrillation be decided to be 0, according to the arbitrary value that microscope records, remaining fiber is between 0-10.
Then form grade scale with the fiber of measuring. Fibrillation value for the fiber of determining any other sample with the naked eye compares the fiber of 5 or 10 fibers and standard class at microscopically. The numerical value of each fiber of then naked eyes being determined averages, and provides the fibrillation value of test sample. It should be understood that these naked eyes are determined and equalization than measuring fast a lot of times, and have found that the fibre technology technical staff of ripe refining is to the classification results self-consistentency of fiber.
The available fiber of extracting out from fabric face is evaluated the fibrillation value of fabric.F.I. the outward appearance of the woven and knitting fabric more than about 2.0-2.5 is unbecoming.
The lyocell fiber of a branch of 1.7 dtexs is wound up and be cut into the staple fibre of 30mm, be spun into 20 spies' yarn then.Yarn is weaved into the wide jersey of 80mm, then that this fabric is concise and dye navy blue.With washing machine with braided fabric 40 ℃ of washings and with family expenses roller drying machine drying.After washing and the dyeing or after circulating, use the fiber of extracting out from the surface of dry fabric to measure fibrillation value (F.I.) through one or more washing/drum dried (W/T).
The mensuration of test method 3-cuoxam viscosity and D.P.
This test is undertaken by TAPPI standard T206 os-63.Cellulose dissolution in the cuoxam that contains 15 ± 0.1g/l copper and 200 ± 5g/l ammoniacal liquor, nitrous acid content＜0.5g/l (Shirley Institute standard), is accurately known the solution of cellulose concentration (about 1%).Measure solution 20 ℃ of times of flowing through tin Lay viscosimeter, the available standards method is calculated viscosity thus.Use following empirical equation to determine sticking equal D.P. value:
D.P.＝412.4285?ln〔100(t-k/t)/n.C〕-348
In the formula, t is a flowing time, shows with stopwatch, and k is a gravity constant, and C is the viscometer tube constant, and n is the water density under test temperature, represents (20 ℃ time, be 0.9982) with g/ml.
The present invention will be described below in conjunction with embodiment, and except that particularly pointing out, part and ratio are by weight.Embodiment 1
Preparation contains the spinning solution of (various ratios, the various degree of polymerization (D.P.)) cellulose, 74-80%NMMO and the 7.5-12.6% water that below will illustrate.This stoste is extruded with having the spinning head that 95 diameters respectively are the hole of 80 μ m (115 ℃ of head temperatures), with the space of the length of explanation, entered in 25 ℃ the spinning bath that contains 25%NMMO and 75% water, form the lyocell fiber by below.Be blown into air from last supply port and following supply port, allow air laterally blow over the filament of extruding.The degree of depth that the zone is promptly gone up in these cross-flow the 1st zones is about 4mm.The 2nd crossflow promptly descends crossflow to be blown into air flow and to form from the moulding funnel with the hand electric hair-dryer.As required, can be by a spot of low-pressure steam being released into cross-flow moisture under the air supply port of funnel inlet increases, thus increase relative humidity (R.H.).The washing fiber is removed residual NMMO, and is dry then.Then be inclined to the fibrillation of test method 1 evaluation fiber.With fiber sample cutting short-forming fiber and spun yarn.Press grade 1 (very poor) to 5 (fine) visual appraisal yarn qualities.The experiment detailed content and the results are shown in Table 1:
Table 1
Cellulose % cellulose D.P. yarn qualities filament bonding
C
f(TM1) spinning speed: 60m/min; Space: 20mm; Last air feed (the 1st zone): 20 ℃/0%R.H.; Following air feed (the 2nd zone): 20 ℃/40%R.H.
15 850 4 5.5 do not have
15 630 5 6.5 do not have
15 472 5 9.4 do not have
12.5 630 4 5.9 do not have
10 850 4 5.3 no spinning speed: 30m/min; Space: 75mm; Last air feed (the 1st zone): 20 ℃/0 % R.H.; Following air feed (the 2nd zone): 20 ℃/40 % R.H.
15 850 4 6.6 do not have
15 630 5 4.9 do not have
15 472 4 3.3 some
12.5 630 3 4.1 some
10 850 4 4.2 no spinning speed: 30m/min; Space: 150mm; Last air feed (the 1st zone): 20 ℃/40 % R.H.; Following air feed (the 2nd zone): 30 ℃/60 % R.H.
15 850 3 3.2 some
15 630 3 0.0 seldom
15 472 2 0.1 bondings
12.5 630 1 0.0 bondings
10 850 1 2.5 bonding spinning speed: 10m/min; Space: 150mm; Last air feed (the 1st zone): 20 ℃/0 % R.H.; Following air feed (the 2nd zone): 20 ℃/40 % R.H.
15 850 4 3.8 seldom
15 630 2 1.3 is serious
15 472 2 0.1 some
12.5 630 1 0.7 bondings
10 850 1 3.5 bonding spinning speed: 10m/min; Space: 75mm; Last air feed (the 1st zone): 20 ℃/40 % R.H.; Following air feed (the 2nd zone): 30 ℃/60 % R.H.
15 850 4 0.0 do not have
15 630 3 1.5 is few
15 472 2 0.0 bondings
12.5 630 1 2.1 bondings
10 850 1 4.8 bonding embodiment 2
Repeat embodiment 1, institute's difference is that stoste contains 15.2% wood pulp cellulose (D.P.600), 75%NMMO and 9.8% water.Evaluate the fibrillation tendency of the fiber that makes thus with test method 1 and 2.Experiment content and the results are shown in Table 2:
Table 2
Air ℃/R.H.% spinning quality C
f(TM1) fiber F.I. (TM2) goes up air feed bonding washing/dyeing 1W/T spinning speed under the air feed: 60m/min; Space: 20mm
-20,/40 5 11.0 does not have 4.7 5.5
-30,/60 5 9.0 does not have 4.7 6.0 spinning speeds: 30m/min; Space: 150mm
-30,/60 3.0 0.1 has 1.7 4.1 20,/40 30,/60 2.7 1.7 1.9 1.9 spinning speeds: 10m/min is arranged; Space: 75mm
-30,/60 3.3 3.6 some 2.5 3.5 60,/40 30,/60 4.0 0.7 nothing 1.0 2.0 spinning speeds: 10m/min; Space: 150mm
-20,/40 1.3 1.2 serious-2,0/0 20,/40 2.0 3.1 has 2.7 5.2
In 110 ℃ of experiments of carrying out the 20mm space of spinneret temperature.Carry out the more experiment in vast sky crack for 90,100 and 110 ℃ in the spinneret temperature; Between these results, only observe little difference, these results are averaged.Embodiment 3
Repeat embodiment 1, institute's difference is that the temperature of last air feed and relative humidity are 20 ℃ and 40%, and air feed is 30 ℃ and 60% down.Other experiment contents and the results are shown in Table 2:
Table 3
| Cellulose D.P. | Cellulose (%) | Spinning speed (m/min) | Space (mm) | Air speed (m/min) | Tow tension | Stability of spinning process | ????C f |
| ???630 | ???15 | ????10 | ???20 | ????2 | ????44 | Good | ????3.8 |
| ???630 | ???15 | ????10 | ???20 | ????8 | ????53 | Good | ????1.9 |
| ???630 | ???15 | ????10 | ???40 | ????2 | ????25 | Difference | ????0.0 |
| ???630 | ???15 | ????10 | ???40 | ????8 | ????52 | Good | ????0.0 |
| ???630 | ???15 | ????10 | ???80 | ????2 | ????45 | Good | ????0.0 |
| ???630 | ???15 | ????20 | ???20 | ????2 | ????100 | Good | ????7.1 |
| ???630 | ???15 | ????20 | ???20 | ????8 | ????165 | Good | ????6.4 |
| ???630 | ???15 | ????20 | ???40 | ????2 | ????80 | Difference | ????5.8 |
| ???630 | ???15 | ????20 | ???40 | ????8 | ????148 | Good | ????3.0 |
| ???630 | ???15 | ????20 | ???80 | ????2 | ????69 | Qualified | ????2.1 |
| ???630 | ???15 | ????40 | ???20 | ????2 | ????120 | Fine | ????10.6 |
| ???630 | ???15 | ????40 | ???20 | ????8 | ????150 | Fine | ????9.5 |
| ???630 | ???15 | ????40 | ???40 | ????2 | ????150 | Fine | ????6.2 |
| ???630 | ???15 | ????40 | ???40 | ????8 | ????225 | Fine | ????6.0 |
| ???630 | ???15 | ????40 | ???80 | ????2 | ????126 | Good | ????5.4 |
| Cellulose D.P. | Cellulose (%) | Spinning speed (m/min) | Space (mm) | Air speed (m/min) | Tow tension | Stability of spinning process | ????C f |
| ????850 | ???13 | ?????10 | ???20 | ????2 | ?????57 | Fine | ????5.1 |
| ????850 | ???13 | ?????10 | ???20 | ????8 | ?????84 | Fine | ????3.0 |
| ????850 | ???13 | ?????10 | ???40 | ????2 | ?????65 | Qualified | ????2.2 |
| ????850 | ???13 | ?????10 | ???40 | ????8 | ?????151 | Good | ????0.2 |
| ????850 | ???13 | ?????20 | ???20 | ????2 | ?????110 | Fine | ????5.5 |
| ????850 | ???13 | ?????20 | ???20 | ????8 | ?????117 | Fine | ????1.0 |
| ????850 | ???13 | ?????20 | ???40 | ????2 | ?????90 | Good | ????4.5 |
| ????850 | ???13 | ?????20 | ???40 | ????8 | ?????256 | Good | ????6.0 |
| ????850 | ???13 | ?????40 | ???20 | ????2 | ?????140 | Fine | ????8.9 |
| ????850 | ???13 | ?????40 | ???20 | ????8 | ?????170 | Fine | ????6.8 |
| ????850 | ???13 | ?????40 | ???40 | ????2 | ?????130 | Good | ????7.1 |
| ????850 | ???13 | ?????40 | ???40 | ????8 | ?????340 | Good | ????6.0 |
| ????850 | ???13 | ?????40 | ???80 | ????2 | ?????110 | Qualified | ????5.4 |
| Cellulose D.P. | Cellulose (%) | Spinning speed (m/min) | Space (mm) | Air speed (m/min) | Tow tension | Stability of spinning process | ????C f |
| ????850 | ???15 | ????10 | ????20 | ????2 | ????240 | Fine | ????2.7 |
| ????850 | ???15 | ????10 | ????20 | ????8 | ????650 | Good | ????1.4 |
| ????850 | ???15 | ????10 | ????40 | ????2 | ????250 | Fine | ????0.0 |
| ????850 | ???15 | ????10 | ????40 | ????8 | ????920 | Difference | ????1.3 |
| ????850 | ???15 | ????10 | ????80 | ????2 | ????220 | Good | ????0.6 |
| ????850 | ???15 | ????10 | ????160 | ????2 | ????310 | Qualified | ????0.0 |
| ????850 | ???15 | ????20 | ????20 | ????2 | ????300 | Fine | ????5.8 |
| ????850 | ???15 | ????20 | ????20 | ????8 | ????900 | Difference | ????6.0 |
| ????850 | ???15 | ????20 | ????40 | ????2 | ????220 | Fine | ????2.4 |
| ????850 | ???15 | ????20 | ????40 | ????8 | ????900 | Difference | ????2.0 |
| ????850 | ???15 | ????20 | ????80 | ????2 | ????220 | Fine | ????0.2 |
| ????850 | ???15 | ????20 | ????80 | ????8 | ????280 | Good | ????0.2 |
| ????850 | ???15 | ????40 | ????20 | ????2 | ????460 | Fine | ????4.6 |
| ????850 | ???15 | ????40 | ????20 | ????8 | ????1000 | Difference | ????5.8 |
| ????850 | ???15 | ????40 | ????40 | ????2 | ????290 | Fine | ????5.4 |
| ????850 | ???15 | ????40 | ????40 | ????8 | ????800 | Qualified | ????5.0 |
| ????850 | ???15 | ????40 | ????80 | ????2 | ????210 | Fine | ????0.0 |
Tow tension is an arbitrary value, and higher numerical value shows bigger tension force.When the space is longer, observe the filament of some adhesions sometimes, especially when air speed is higher.Embodiment 4
Preparation contains the spinning solution of 13% cellulose (average D.P.800), 75%NMMO and 12% water.With this stoste (former liquid temp is 83 ℃) with having 18, the spinning head that 400 diameters respectively are 70 μ m, be clustered in three holes that list arranged side by side that respectively are about 1m is extruded, by the long space of 30mm, enter in the spinning bath that contains 25%NMMO and 75% water, form the lyocell fibre bundle.Allow the air of supply of two supply ports laterally blow over fibre bundle, the last air supply opening of next-door neighbour's spinning head is from the blowing nozzle of the 5mm speed air feed with 12m/sec, and the following air supply opening that is positioned at the bottom, space is from the blowing nozzle of the 25mm speed air feed with 9m/sec.Bleed with identical speed by the suction nozzle that is positioned at each blowing nozzle opposite.The temperature of last air feed (relatively dry) is 20 ℃, and its relative humidity is 40% (dew point is 6 ℃).The temperature of following air feed (moistening relatively) is 28 ℃, and its relative humidity is 78% (dew point is 24 ℃).Spinning quality and having good stability.Close then and close air supply opening.Spinning quality is variation immediately, needs to recover to go up air feed rapidly and damages (losing stability of spinning process) to avoid the fibre bundle in the spinning bath.
Claims (14)
1.lyocell the manufacture method of extruded product, wherein, extrude with the cellulose solution that shower nozzle will be dissolved in the N-tertiary amine oxide, by entering behind the space in the spinning bath, supply air in the space and and extract out from the space, it is characterized in that the space comprises with contiguous the 1st zone of the face of shower nozzle with from the face of shower nozzle the 2nd zone far away, the moisture that is conducted to the air in the 1st zone remains below the level of the moisture of the air that is conducted to the 2nd zone.
2. the method for claim 1 is characterized in that, gap lengths is preferably between the 20-60mm between 10-160mm.
3. method as claimed in claim 1 or 2 is characterized in that the length in the 1st zone is less than the length in the 2nd zone.
4. method as claimed in claim 3 is characterized in that the length in the 1st zone is between 3-10mm.
5. the method according to any one of the preceding claims is characterized in that, is conducted to any speed of air in the 1st zone and the 2nd zone between 1-20m/sec, is preferably between the 2-10m/sec.
6. the method according to any one of the preceding claims is characterized in that, with air to be conducted to the 1st zone and the 2nd zone with the horizontal substantially direction of the direct of travel of extrudate by the space.
7. the method according to any one of the preceding claims is characterized in that, with blowing nozzle with air be conducted to the space the 1st the zone and the 2nd zone, above-mentioned blowing nozzle is located at two zones respectively.
8. method as claimed in claim 7 is characterized in that, uses towards the single suction nozzle of blowing nozzle air is discharged from the space.
9. method as claimed in claim 7 is characterized in that, uses towards blowing nozzle that respectively separates and the suction nozzle that separates with identical size and discharges air.
10. the method according to any one of the preceding claims is characterized in that, the moisture that is conducted to the air in the 2nd zone is higher than the moisture of the air that is conducted to the 1st zone, and its difference is preferably between 10-20g water/kg air between 1-30g water/kg air.
11. the method according to any one of the preceding claims is characterized in that, the moisture of air that is conducted to the 1st zone is preferably between 0-10g water/kg air between 0-20g water/kg air.
12. the method according to any one of the preceding claims is characterized in that, the moisture of air that is conducted to the 2nd zone is between 5-30g water/kg air.
13. the method according to any one of the preceding claims is characterized in that, the cellulosic average degree of polymerization in the solution is between 750-1000.
14. the method according to any one of the preceding claims is characterized in that, extruded product is the form of lyocell long filament.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB9500387.7 | 1995-01-10 | ||
| GBGB9500387.7A GB9500387D0 (en) | 1995-01-10 | 1995-01-10 | Manufacture of extruded articles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1168159A true CN1168159A (en) | 1997-12-17 |
Family
ID=10767787
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96191362A Pending CN1168159A (en) | 1995-01-10 | 1996-01-09 | Manufacture of extruded articles |
Country Status (13)
| Country | Link |
|---|---|
| EP (1) | EP0802992A1 (en) |
| JP (1) | JPH10505886A (en) |
| KR (1) | KR19980701273A (en) |
| CN (1) | CN1168159A (en) |
| AU (1) | AU4351496A (en) |
| BR (1) | BR9606733A (en) |
| CZ (1) | CZ206697A3 (en) |
| FI (1) | FI972465A (en) |
| GB (1) | GB9500387D0 (en) |
| SK (1) | SK84197A3 (en) |
| TR (1) | TR199700597T1 (en) |
| TW (1) | TW303395B (en) |
| WO (1) | WO1996021758A1 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1325704C (en) * | 2001-08-11 | 2007-07-11 | 莱恩真纤维有限公司 | Precipitating bath |
| CN1329564C (en) * | 2002-05-24 | 2007-08-01 | 齐默尔股份公司 | Wetting unit and spinning equipment with wetting unit |
| CN101292063B (en) * | 2005-08-23 | 2011-03-23 | 连津格股份公司 | Multiple spinning nozzle arrangement and method for suctioning and blowing |
| CN102477591A (en) * | 2010-11-19 | 2012-05-30 | 中国纺织科学研究院 | Cellulose fiber, and manufacturing method and equipment thereof |
| CN101235580B (en) * | 2006-12-22 | 2013-03-27 | 赖芬豪泽机械工厂有限及两合有限公司 | Method and device for the manufacture of a spunbonded fabric of cellulosic filaments |
| CN110234802A (en) * | 2017-03-27 | 2019-09-13 | 东丽株式会社 | The manufacturing method of fiber and the manufacturing method of carbon fiber |
Families Citing this family (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB9605504D0 (en) * | 1996-03-15 | 1996-05-15 | Courtaulds Plc | Manufacture of elongate members |
| GB9607456D0 (en) * | 1996-04-10 | 1996-06-12 | Courtaulds Fibres Holdings Ltd | Spinning of filaments |
| GB2319495A (en) * | 1996-11-26 | 1998-05-27 | Courtaulds Fibres | Method and apparatus for the manufacture of lyocell fibres |
| DE19717257A1 (en) * | 1997-04-24 | 1998-10-29 | Akzo Nobel Nv | Method of manufacturing cellulosic bodies using coagulation bath |
| AT405531B (en) | 1997-06-17 | 1999-09-27 | Chemiefaser Lenzing Ag | METHOD FOR PRODUCING CELLULOSIC FIBERS |
| DE19954152C2 (en) * | 1999-11-10 | 2001-08-09 | Thueringisches Inst Textil | Method and device for producing cellulose fibers and cellulose filament yarns |
| DE10190965D2 (en) * | 2000-03-11 | 2003-05-08 | Thueringisches Inst Textil | Method and device for producing cellulose fibers and cellulose filament yarns |
| DE10043297B4 (en) * | 2000-09-02 | 2005-12-08 | Thüringisches Institut für Textil- und Kunststoff-Forschung e.V. | Process for the production of cellulose fibers and cellulose filament yarns |
| DE10206089A1 (en) | 2002-02-13 | 2002-08-14 | Zimmer Ag | bursting |
| AT412728B (en) * | 2002-09-03 | 2005-06-27 | Chemiefaser Lenzing Ag | CELLULOSE FIBER |
| KR100966111B1 (en) * | 2005-03-15 | 2010-06-28 | 주식회사 효성 | Manufacturing method of cellulose multifilament |
| KR100824980B1 (en) * | 2006-12-28 | 2008-04-28 | 주식회사 효성 | Cellulose Multifilament with Low Cross Section Coefficient |
| EP2565304A1 (en) * | 2011-09-02 | 2013-03-06 | Aurotec GmbH | Extrusion method and device |
| KR101455002B1 (en) | 2013-06-28 | 2014-11-03 | 코오롱인더스트리 주식회사 | Lyocell Material Cigarette Filter and Method for the Same |
| US10306919B2 (en) | 2013-09-26 | 2019-06-04 | Kolon Industries, Inc. | Lyocell material for cigarette filter and method for preparing same |
| TWI667378B (en) | 2014-01-03 | 2019-08-01 | 奧地利商蘭精股份有限公司 | Cellulosic fibre |
| KR102205529B1 (en) * | 2014-03-31 | 2021-01-20 | 코오롱인더스트리 주식회사 | Lyocell Fiber |
| KR102211219B1 (en) | 2014-06-30 | 2021-02-03 | 코오롱인더스트리 주식회사 | Lyocell Material with Noncircle Cross Section for Cigarette Filter And Manufacturing Method of the same |
| KR102211186B1 (en) | 2014-12-31 | 2021-02-03 | 코오롱인더스트리 주식회사 | Lyocell Material Cigarette Filter and Method for the Same |
| EP3470557A1 (en) * | 2017-10-12 | 2019-04-17 | Lenzing Aktiengesellschaft | Spinning device and method for stringing up in a spinning device |
| EP3674454A1 (en) * | 2018-12-28 | 2020-07-01 | Lenzing Aktiengesellschaft | Cellulose filament process |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ATA53792A (en) * | 1992-03-17 | 1995-02-15 | Chemiefaser Lenzing Ag | METHOD FOR PRODUCING CELLULOSIC MOLDED BODIES, DEVICE FOR IMPLEMENTING THE METHOD AND USE OF A SPINNING DEVICE |
| MY115308A (en) * | 1993-05-24 | 2003-05-31 | Tencel Ltd | Spinning cell |
| AT399729B (en) * | 1993-07-01 | 1995-07-25 | Chemiefaser Lenzing Ag | METHOD FOR PRODUCING CELLULOSIC FIBERS AND DEVICE FOR IMPLEMENTING THE METHOD AND THE USE THEREOF |
| AT402738B (en) * | 1993-07-28 | 1997-08-25 | Chemiefaser Lenzing Ag | SPIDER NOZZLE |
-
1995
- 1995-01-10 GB GBGB9500387.7A patent/GB9500387D0/en active Pending
-
1996
- 1996-01-09 AU AU43514/96A patent/AU4351496A/en not_active Abandoned
- 1996-01-09 JP JP8521509A patent/JPH10505886A/en active Pending
- 1996-01-09 SK SK841-97A patent/SK84197A3/en unknown
- 1996-01-09 CZ CZ972066A patent/CZ206697A3/en unknown
- 1996-01-09 TR TR97/00597T patent/TR199700597T1/en unknown
- 1996-01-09 BR BR9606733A patent/BR9606733A/en not_active Application Discontinuation
- 1996-01-09 EP EP96900125A patent/EP0802992A1/en not_active Ceased
- 1996-01-09 KR KR1019970704662A patent/KR19980701273A/en not_active Application Discontinuation
- 1996-01-09 CN CN96191362A patent/CN1168159A/en active Pending
- 1996-01-09 WO PCT/GB1996/000030 patent/WO1996021758A1/en not_active Application Discontinuation
- 1996-01-11 TW TW085100387A patent/TW303395B/zh active
-
1997
- 1997-06-10 FI FI972465A patent/FI972465A/en unknown
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1325704C (en) * | 2001-08-11 | 2007-07-11 | 莱恩真纤维有限公司 | Precipitating bath |
| CN1329564C (en) * | 2002-05-24 | 2007-08-01 | 齐默尔股份公司 | Wetting unit and spinning equipment with wetting unit |
| CN101292063B (en) * | 2005-08-23 | 2011-03-23 | 连津格股份公司 | Multiple spinning nozzle arrangement and method for suctioning and blowing |
| CN101235580B (en) * | 2006-12-22 | 2013-03-27 | 赖芬豪泽机械工厂有限及两合有限公司 | Method and device for the manufacture of a spunbonded fabric of cellulosic filaments |
| CN102477591A (en) * | 2010-11-19 | 2012-05-30 | 中国纺织科学研究院 | Cellulose fiber, and manufacturing method and equipment thereof |
| CN102477591B (en) * | 2010-11-19 | 2013-12-11 | 中国纺织科学研究院 | Cellulose fiber, preparation method thereof and equipment |
| CN110234802A (en) * | 2017-03-27 | 2019-09-13 | 东丽株式会社 | The manufacturing method of fiber and the manufacturing method of carbon fiber |
| CN110234802B (en) * | 2017-03-27 | 2021-11-26 | 东丽株式会社 | Method for producing fiber and method for producing carbon fiber |
Also Published As
| Publication number | Publication date |
|---|---|
| CZ206697A3 (en) | 1998-01-14 |
| FI972465A (en) | 1997-07-11 |
| WO1996021758A1 (en) | 1996-07-18 |
| KR19980701273A (en) | 1998-05-15 |
| SK84197A3 (en) | 1998-03-04 |
| EP0802992A1 (en) | 1997-10-29 |
| BR9606733A (en) | 1998-01-13 |
| FI972465A0 (en) | 1997-06-10 |
| TR199700597T1 (en) | 1998-01-21 |
| TW303395B (en) | 1997-04-21 |
| JPH10505886A (en) | 1998-06-09 |
| AU4351496A (en) | 1996-07-31 |
| GB9500387D0 (en) | 1995-03-01 |
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