CN109881271B - Method and device for spinning - Google Patents
Method and device for spinning Download PDFInfo
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- CN109881271B CN109881271B CN201910156589.7A CN201910156589A CN109881271B CN 109881271 B CN109881271 B CN 109881271B CN 201910156589 A CN201910156589 A CN 201910156589A CN 109881271 B CN109881271 B CN 109881271B
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- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000009987 spinning Methods 0.000 title claims abstract description 27
- 239000000835 fiber Substances 0.000 claims abstract description 44
- 239000011347 resin Substances 0.000 claims abstract description 42
- 229920005989 resin Polymers 0.000 claims abstract description 42
- 229920000412 polyarylene Polymers 0.000 claims abstract description 40
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 32
- 230000009477 glass transition Effects 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims description 136
- 238000003860 storage Methods 0.000 claims description 39
- 238000010438 heat treatment Methods 0.000 claims description 29
- 230000008569 process Effects 0.000 claims description 12
- 238000012546 transfer Methods 0.000 claims description 8
- 239000003921 oil Substances 0.000 description 161
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 20
- 239000000203 mixture Substances 0.000 description 13
- 239000004734 Polyphenylene sulfide Substances 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 11
- 229920000069 polyphenylene sulfide Polymers 0.000 description 11
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 8
- -1 Polytetrafluoroethylene Polymers 0.000 description 8
- 238000012681 fiber drawing Methods 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- 229920000642 polymer Polymers 0.000 description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 5
- 238000001125 extrusion Methods 0.000 description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- QPFMBZIOSGYJDE-UHFFFAOYSA-N 1,1,2,2-tetrachloroethane Chemical compound ClC(Cl)C(Cl)Cl QPFMBZIOSGYJDE-UHFFFAOYSA-N 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- KZTYYGOKRVBIMI-UHFFFAOYSA-N diphenyl sulfone Chemical compound C=1C=CC=CC=1S(=O)(=O)C1=CC=CC=C1 KZTYYGOKRVBIMI-UHFFFAOYSA-N 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
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- 238000010992 reflux Methods 0.000 description 2
- 150000003568 thioethers Chemical class 0.000 description 2
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
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- 239000004743 Polypropylene Substances 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012784 inorganic fiber Substances 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000006224 matting agent Substances 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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- 238000003303 reheating Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
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- 239000002699 waste material Substances 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
Images
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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
- D01D5/14—Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
-
- 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
- D01D5/12—Stretch-spinning methods
- D01D5/16—Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Textile Engineering (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention relates to a method and a device for spinning, in particular to a method and a device for producing resin with higher glass transition temperature, especially polyarylene sulfide fiber.
Description
Technical Field
The invention belongs to the field of production methods of chemical textile products, particularly relates to a production method and production equipment of a fiber material, and more particularly relates to a production method and a production device of resin with higher glass transition temperature, particularly polyarylene sulfide fiber.
Background
Polyarylene sulfide (PAS) resin has excellent properties suitable as engineering plastics, such as heat resistance, shielding properties, chemical resistance, electrical insulation properties, and moist heat resistance. As a representative of polyarylene sulfide, polyphenylene sulfide (PPS) is widely used in various product processes.
The PPS fiber is a novel special plastic fiber, is prepared by adopting a conventional melt spinning method and performing post-processing and the like on PPS resin (PPS) at high temperature, and comprises filaments, monofilaments, yarns, short fibers and the like. After stretching, the short fiber can be prepared by curling and cutting, and the short fiber has the following properties: the strength is 2.65-3.08 cN/dtex, the elongation is 25-35%, the melting point is 285 ℃, the heat stability and the flame retardance are excellent, the oxygen index value is 34-35, the strength retention rate is 60% at 200 ℃, and the elongation at break is unchanged; second only to Polytetrafluoroethylene (PTFE) fibers; has better spinning processing performance. The product is mainly used for filtering high-temperature flue gas and special heat medium, drying belts in paper industry, cable rubber coating layers, fireproof fabrics and the like, and the woven fabric can be used for manufacturing high-grade fire-fighting clothes.
However, the excellent properties of PPS itself also place new demands on the current process of fiber formation. For example, in spinning, it is necessary to draw a strand fiber in an oil bath to have a desired fineness and orient molecular chains to increase the strength of the fiber. Most synthetic fibers, such as polyamide, polyester and polyolefin, are produced at a temperature of 60 to 80 ℃ during oil bath drawing because of their low glass transition temperature. However, the glass transition temperature of PPS is high, and when the strand is heated and stretched in an oil bath, the temperature is usually set to 90 to 98 ℃.
Generally, a liquid medium in an oil bath is heated in an oil bath low-level tank, conveyed into the oil bath tank through a pump and then reflowed to the oil bath low-level tank for recycling, and when a vehicle is driven or stopped, the height of the liquid level in the oil bath tank is adjusted by controlling a valve for reflowing an oil bath tank to the low-level tank. In the production of PPS fibers, problems arise with this model: 1. because the glass transition temperature of PPS is high, the heating temperature needs to be above 90 ℃, and when the high-temperature liquid medium is pumped into the oil bath from the low tank, cavitation is easy to generate when water or a mixed solvent is used as the medium, and the temperature fluctuation of the liquid medium in the oil bath is usually caused to exceed +/-3 ℃; 2. when the vehicle is driven or stopped, a large amount of high-temperature liquid medium needs to be introduced into or extracted from the oil bath tank by a pump or a valve in a short time, so that the efficiency is low and the vehicle is not economical.
Citation 1 discloses a drawing bath heating device, which comprises a drawing bath with a water inlet and a water outlet, a conduit, an oil boiler, an oil bath and a water pump, wherein the oil boiler is connected with the oil bath through the conduit to form a closed circulating oil path, and heat conducting oil is arranged in the closed oil path; the oil bath groove is respectively connected with the water inlet and the water outlet of the drafting bath groove through guide pipes, and the water pump transfers the water in the oil bath groove and the water in the drafting bath groove through the guide pipes. Although the oil bath tank and the drafting bath tank are separated, so that the temperature in the drafting bath tank is more uniform, and the drafting is convenient to carry out, the water is still required to be heated and then conveyed by a water pump, and the hot water is directly injected into the oil bath tank.
Citation 2 discloses an oil bath tow stretching device, which comprises a front drafting machine roller device, a rear drafting machine roller device and an intermediate heating device, wherein the intermediate heating device is arranged between the front drafting machine roller device and the rear drafting machine roller device, the intermediate heating device is an oil bath groove, two ends of the oil bath groove are respectively provided with an immersion roller, and the immersion rollers are correspondingly provided with a guide roller which is connected with the front drafting machine roller device and the rear drafting machine roller device; the device can prevent mutual bonding of tows, facilitates the shunting and stacking of the tows at the back to be curled, facilitates the disassembly and the maintenance, and can also reduce the generation of waste silk. It does not involve circulation and transport as a heating medium.
Therefore, although various methods have been tried in the art to stabilize the temperature at the time of fiber drawing in the spin-drawing process, there is still room for further improvement in the arrangement of the heating device at the time of fiber drawing and the circulation arrangement as the heating medium.
Cited documents:
cited document 1: CN202380141U
Cited document 2: CN106757434A
Disclosure of Invention
Problems to be solved by the invention
Aiming at the basic situation in the spinning or fiber drawing process in the field, the technical problem to be solved by the invention is how to keep the uniform heating and the accurate and controllable heating temperature in the fiber drawing process in the resin spinning or resin fiber drawing process which needs high-temperature heating, avoid the damage of the high-temperature transmission of the heating medium to the quality of the fiber in an oil bath groove, and avoid the problem of insufficient utilization rate of the heating medium caused by the violent change of the flow of the heating medium when the equipment is started or stopped.
Furthermore, the invention also relates to how to provide a method for producing high quality spun fibers, in particular polyarylene sulfide spun fibers.
Means for solving the problems
Through extensive research by the inventors of the present invention, it was found that the above technical problems can be solved by the following solutions:
[1] the present invention firstly provides a method of resin spinning comprising:
the fibers formed by the resin or the combination thereof are introduced into the liquid medium of the oil bath,
drawing the fibers in the liquid medium,
the liquid medium flows into the oil bath groove from the oil bath storage groove, the liquid medium flowing out from the oil bath groove flows into the low-temperature groove,
the temperature of the liquid medium in the oil bath storage tank is higher than that of the liquid medium in the low-temperature tank,
[2] the method according to [1], wherein the liquid medium is sent from the low-temperature tank to the oil bath storage tank by a transfer pump.
[3] The method according to [1] or [2], wherein the glass transition temperature of the resin is 85 ℃ or higher, and preferably the resin is a polyarylene sulfide resin.
[4] The method according to any one of [1] to [3], wherein the liquid medium is heated in the oil bath storage tank, preferably the liquid medium is heated to 90 ℃ or higher.
[5] The process according to any one of [1] to [4], wherein the temperature of the liquid medium in the oil bath is 90 ℃ or higher;
[6] the method according to any one of [1] to [5], wherein the temperature of the liquid medium in the low-temperature tank is 20 to 80 ℃, preferably 60 to 80 ℃.
[7] Further, the present invention also provides an oil bath for resin spinning, comprising:
an oil bath groove is formed in the bottom of the tank body,
the oil bath storage tank is arranged in the oil bath tank,
a low-temperature groove is arranged on the upper surface of the shell,
the oil bath groove, the oil bath storage tank and the low-temperature groove are connected with a valve through pipelines.
[8] The device of claim 7, wherein the glass transition temperature of the resin is 85 ℃ or higher, preferably wherein the resin is a polyarylene sulfide resin.
[9] The apparatus according to [7] or [8], further comprising a transfer pump for transferring a liquid medium which is sent from the low-temperature bath into the oil bath storage tank by the transfer pump.
[10] The apparatus according to any one of [7] to [9], wherein the oil bath tank has a heating means for heating the liquid medium, the liquid medium is heated in the oil bath tank by the heating means, and preferably the liquid medium is heated to 90 ℃ or higher.
[11] The apparatus according to any one of [7] to [10], wherein a draft roller is further provided in the oil bath.
[12] The apparatus according to any one of [7] to [11], wherein the liquid medium flows from the oil bath reservoir into the oil bath, and the liquid medium flowing out from the oil bath flows into the low-temperature tank.
ADVANTAGEOUS EFFECTS OF INVENTION
By using the method of the present invention, the following beneficial technical effects can be obtained in the process of spinning or fiber preparation of the polyarylene sulfide:
1) compared with the existing oil bath equipment, the oil bath equipment has the advantages that the independent oil bath storage tank is introduced, the liquid medium for oil bath is heated in the oil bath storage tank, the heated liquid medium is sent into the oil bath through the valve, and the situation that the hot liquid medium is directly sent into the oil bath by the pump is avoided.
2) The heating temperature of the liquid medium in the oil bath storage tank is easy to control, and the liquid medium can flow into the oil bath tank at a stable flow rate through a valve, so that the influence on the quality of the fiber caused by the aggravation of thermal convection in the oil bath tank can be avoided. Also, the temperature in the oil bath can be controlled more accurately by controlling the flow rate or flow rate of the hot liquid medium flowing into the oil bath.
3) Unlike the prior art in which the liquid medium is heated in the lower tank (at a temperature close to or slightly higher than the treatment temperature preset in the oil bath), the liquid medium may be not heated or only appropriately preheated (at a temperature not exceeding 80 ℃) in the lower tank in the present invention, and therefore, the prior art lower tank is also referred to as a low-temperature tank in the present invention. The liquid medium with low temperature is conveyed from the low-temperature tank through the pump, so that the high-temperature loss of the pump when the pump is used for conveying the high-temperature medium in the traditional process is avoided; meanwhile, the heating efficiency is increased, and a large amount of high-temperature liquid medium can be introduced into the oil bath groove in a short time.
Drawings
FIG. 1: a prior art representation of an oil bath for use in polyarylene sulfide spinning or fiber drawing;
FIG. 2: a representation of an oil bath for use in the present invention in polyarylene sulfide spinning or fiber drawing.
In the above illustration: the left side is a plan view and the right side is a front view.
Detailed Description
The resin spinning method and the apparatus thereof according to the present invention will be described in detail below. It is to be noted that, unless otherwise specified, the unit names used in the present invention are all international unit names commonly used in the art. Furthermore, the recitation of numerical values or ranges of values herein below is understood to include industry-accepted errors.
< first aspect of the invention >
The first aspect of the present invention relates to a method for spinning a resin, and the kind of such a resin is not particularly limited as long as the glass transition temperature of the resin is 85 ℃ or higher, preferably 90 ℃ or higher. The first aspect of the present invention is particularly suitable for spinning polyarylene sulfide resins and compositions thereof. More particularly, in some specific embodiments, the invention relates to a method of drawing polyarylene sulfide fibers in an oil bath.
Polyarylene sulfide or composition thereof
The repeating unit of the chain structure of Polyarylene Sulfide (PAS) is- [ -Ar-S- ] -or a high molecular polymer having a segment of the repeating unit, and the high molecular polymer mainly comprising aryl and Sulfide structures in the main chain structure of the molecule is generally called. The polymer has a series of excellent properties; such as excellent heat resistance, chemical resistance, radiation resistance, flame retardancy, excellent mechanical and electrical properties, dimensional stability, etc.
The polyarylene sulfide suitable for use in the present invention is not particularly limited, and various polyarylene sulfides generally suitable for spinning in the art can be used. The polyarylene sulfide according to the present invention, without limitation, may be selected from any one or more of polyphenylene sulfide, polyarylene sulfide sulfone, polyarylene sulfide ketone, polyarylene sulfide nitrile, polyarylene sulfide amide, polyarylene sulfide sulfone amide, polyarylene sulfide ketone amide, or copolymer of polyphenylene sulfide in any proportion.
The weight average molecular weight of the polyarylene sulfide resin which can be used in the present invention is not particularly limited, and in some preferred embodiments, it may beIs 2.0X 104Above, 4.0 × 104Above, 6.0 × 104Above, and typically 10.1 × 104The following.
In some specific embodiments, the polyarylene sulfide according to the present invention may be used in combination with other resins, such as polyamide, polyimide, phenolic resin, etc. having compatibility with the polyarylene sulfide, as needed, in addition to the above-mentioned polymers, to form a composition. Preferably, the polyarylene sulfide according to the present invention may contain, in addition to the polyarylene sulfide itself, other resins in an amount of not more than 40% based on the total mass of the mixture or the composition.
In other specific embodiments, fillers, which may be inorganic particles, chopped fibers, etc., may also be used as reinforcing components in the polyarylene sulfides described in the present invention. The chopped fibers may be organic fibers or inorganic fibers, such as glass fibers and carbon fibers.
In addition, without limitation, the polyarylene sulfide in the present invention may further contain various functional auxiliaries. For example, the functional adjuvant may be selected from one or more of antioxidants, antistatic agents, softeners, brighteners, light stabilizers, dyes or matting agents.
Spinning
The spinning according to the present invention may be carried out by means of spinning or extrusion equipment which is generally used in the art, and if necessary, by means of or using an organic solvent.
The organic solvent in the present invention is at least one or a mixture of two or more of dimethyl sulfoxide, sulfolane, diphenyl sulfone, N-methyl pyrrolidone, N-dimethylformamide, dimethylacetamide, cyclohexanone and tetrachloroethane. In a preferred embodiment, the present invention may be practiced without these organic solvents.
In some specific embodiments, the polyarylene sulfide or a composition thereof is spun by melting or by means of a solvent. For example, the polyarylene sulfide or a composition thereof is extruded from a spinneret by heating to form a fiber.
In other specific cases, the polyarylene sulfide resin as a spinning raw material or a composition thereof may be mixed with optional additives and fed into an extruder to be subjected to blending extrusion. The polyarylene sulfide resin or its composition can be extruded using an extruder which is generally used in the art for processing polyarylene sulfide resins. The extruder is not particularly limited, but from the viewpoint of extrusion efficiency, a screw extruder is preferably used, and a twin-screw extruder is more preferably used.
The temperature of each section in the extruder is set as 150 ℃ in one zone, 180 ℃ in two zones, 300 ℃ in two zones, and 180 ℃ in three zones, 350 ℃ in three zones, and the temperature of the outlet die of the extruder is 190 ℃ in 320 ℃ in one zone, and preferably is 300 ℃ in 250 ℃ in one zone. In some preferred embodiments of the invention, the extrusion rate is from 0.1 to 2m/s, preferably from 0.5 to 1 m/s.
Oil bath drawing
In the spinning, fibers are prepared through a spinneret or an extruder die, and the fibers are guided into an oil bath groove through a drawing roller to be further stretched.
The fiber is drawn by one or more draw rolls disposed in an oil bath, and immersed in the liquid medium in the oil bath. The liquid medium is not particularly limited, and includes various solvents and substances for surface treatment of the fibers. As the solvent, it may be selected from various solvents having a boiling point of 85 ℃ or higher, preferably 90 ℃ or higher, and may be selected from one or more of water, NMP, DMF, DMSO, DMAc, or triethylene glycol, generally according to need; water or an aqueous phase blending solvent is preferred, the aqueous phase blending solvent being a blending solvent of water and one or more of NMP, DMF, DMSO, DMAc, triethylene glycol, and the like, more preferably water. The surface-treated material is not particularly limited, and various commercially available materials for treating the surface of the fiber, for example, a finishing agent, can be used.
The temperature of the liquid medium in the oil bath is not particularly limited as long as the temperature is not lower than the glass transition temperature Tg of the stretched polyarylene sulfide or a composition thereof. In some particular embodiments of the invention, the temperature of the liquid medium in the oil bath is above 90 ℃, preferably above 95 ℃, optionally the oil bath also having heating means. Since the temperature of the liquid medium is higher than the glass transition temperature of the drawn resin or resin composition, the above fibers can be drawn and drawn in an oil bath. The drawing speed of the drawing rolls is not particularly limited, and fibers having different drawing effects can be obtained by setting different speeds of the plurality of drawing rolls, and the number of the drawing rolls can be set as required according to the required fineness of the fibers. In the present invention, the fineness of the fiber obtained by drawing with the drawing roll may be in the range of 0.8 to 6.0D, preferably 1.0 to 5.0D.
In the present invention, the fiber obtained after spinning or extrusion may be drawn in at least one of the above-mentioned oil bath grooves, and in some specific embodiments, the same or different oil bath grooves may be provided.
The oil bath groove is provided with an inlet and an outlet of the liquid medium. The outlet of the liquid medium of the oil bath groove is connected with the low-temperature groove through a valve and a pipeline, and the inlet of the liquid medium of the oil bath groove is connected with the oil bath storage tank through a valve and a pipeline. The rate of flow of the liquid medium into and out of the oil bath is controlled by the outlet, inlet valves and the temperature of the liquid medium in the oil bath can be controlled thereby.
In some specific embodiments, the outlet is provided at the bottom of the oil bath from which the low temperature liquid medium is drained out of the oil bath by cold-hot convection of the medium, for example when the level of the liquid medium in the oil bath exceeds a standard due to the liquid medium flowing into the oil bath from the oil bath reservoir, the valve at the outlet at the bottom of the oil bath is opened and the liquid medium inlet valve of the oil bath can be closed.
In other specific embodiments, the outlet is positioned above and immediately adjacent to the standard line of the bath liquid medium, and excess liquid medium is automatically drained from the outlet when the level of the liquid medium in the bath exceeds the standard line.
Preferably, the bath may have one or more outlets for the liquid medium, which may be located at the bottom and above the bath liquid medium level gauge line, respectively. Similarly, the oil bath can also have one or more liquid medium inlets, and the liquid medium inlets can be connected with one oil bath storage tank through pipelines or can be respectively connected with a plurality of oil bath storage tanks through pipelines. The position of the liquid medium inlet is not particularly limited, but the inlet may be provided as close as possible to the middle of the oil bath from the viewpoint of controlling the temperature balance of the liquid medium in the oil bath, or the inlet may be provided as a position-movable inlet to uniformly deliver the high-temperature liquid medium to each part of the oil bath by regular reciprocating motion, or when a plurality of inlets are provided, the inlets may be uniformly distributed at different positions of the oil bath.
Without limitation, the oil bath may also have other auxiliary arrangements, such as liquid media agitators, holding devices, etc.
The cryogenic liquid medium in the oil bath is introduced into the cryogenic tank through valves and piping, which in some embodiments may be located below the oil bath and may also be generally referred to as the lower tank. The cold sink contains used or excess liquid medium that has a relatively low temperature relative to the liquid medium in the oil bath. In some embodiments, the temperature of the liquid medium in the cryogenic tank may be maintained between 20 ℃ and 80 ℃, preferably between 60 ℃ and 80 ℃. Optionally, a holding device or a temperature heating device may be provided in the low-temperature tank so that the temperature of the liquid medium is maintained within the above temperature range, and if the temperature is too low, more energy is required for reheating the low-temperature liquid medium when the low-temperature liquid medium is transferred to the oil bath storage tank by the subsequent pump, and if the temperature is too high, the pump is inevitably used to transfer the high-temperature liquid medium, and the loss of the pump may be increased.
When the high-temperature liquid medium flows into the oil bath from the oil bath storage tank, the oil bath storage tank needs to be supplemented with the liquid medium, and at this time, the low-temperature liquid medium in the low-temperature tank is conveyed into the oil bath storage tank through a pipeline by a pump and is heated to 90 ℃ or higher, preferably 95 ℃ or higher in the oil bath storage tank.
The circulation use of the liquid medium is realized through the flow of the liquid medium.
In the invention, through the arrangement of the oil bath storage tank, the defects caused by directly heating the liquid medium in a low-level tank (corresponding to the low-temperature tank of the invention) to a high temperature of more than 90 ℃ and then directly adding the high-temperature liquid medium into the oil bath tank through a pump in the traditional design are avoided. On the one hand, can avoid using the pump to transmit high temperature liquid medium, avoided the mechanical loss of pump like this, on the other hand, the liquid medium input of pump transmission is to the oil bath storage tank, and the oil bath storage tank plays the cushioning effect, can avoid opening at every pump stop the problem that the transmission of liquid medium that causes in the twinkling of an eye is unstable, is difficult to control, also can avoid because the emergence of cavitation that the conveying of high temperature liquid medium leads to. The oil bath storage tank can be used as a buffer to avoid the instable flow of the instantaneous liquid medium, and the high-temperature liquid medium can be conveyed into the oil bath tank at a stable flow rate at any moment through a valve of the oil bath storage tank, so that the temperature of the liquid medium in the oil bath tank can be controlled more accurately. In a preferred embodiment of the present invention, the temperature fluctuation of the liquid medium in the oil bath can be controlled within. + -. 1 ℃ by the above-mentioned method.
< second aspect of the invention >
A second aspect of the present invention relates to an oil bath for spinning resin, the resin being selected as in the first aspect of the present invention. The device comprises:
an oil bath tank, an oil bath storage tank and a low-temperature tank.
The resin fibers are treated by the liquid medium in an oil bath. The liquid medium flows into the oil bath groove from the oil bath storage tank, and the liquid medium flowing out of the oil bath groove flows into the low-temperature groove.
The existing process for fiber drawing using an oil bath is shown in schematic 1. Typically, in the spinning process of terylene or polypropylene and the like, the liquid medium in the oil bath has a certain temperature, the function of the liquid medium is to stretch the protofilament in the bath to reach a certain fineness, and the liquid medium in the oil bath is utilized to protect the surface of the polymer so as to prevent the polymer from causing a large number of defects during stretching and being unfavorable for subsequent processing.
Because the temperature used for oil bath heating is lower and is about 60-80 ℃, the liquid medium heated in the low-level tank (corresponding to the low-temperature tank of the invention) can be pumped into the oil bath tank by a pump, and a valve is opened at one end of the oil bath tank to return the redundant liquid medium to the low-level tank for reuse. By means of the internal circulation, the tows in the oil bath groove are always below the liquid level, and the heating and stretching can be normally carried out.
Therefore, in the prior art, the liquid medium is generally heated in a low-level tank, and the heated liquid medium is directly fed into an oil bath tank by an oil pump. As described above, with such an oil bath design, if it is used directly for drawing of a resin having a higher glass transition temperature, such as polyarylene sulfide resin fibers, there are problems as already explained above, and in particular, if the liquid medium is heated in such a low tank to a temperature equal to or slightly higher than the temperature required in the oil bath and the hot liquid medium is directly fed into the oil bath by pumping, it usually results in a fluctuation in the temperature of the liquid medium in the oil bath by more than ± 3 ℃.
In the apparatus of the present invention, in contrast to the prior art, before the liquid medium in the low-temperature bath is transferred to the oil bath by the pump, the liquid medium is transferred to the oil bath tank and heated in the oil bath tank to a temperature which is the same as or slightly higher than the temperature required in the oil bath, for example, 90 ℃ or higher. As shown in fig. 2, the oil bath in the apparatus of the present invention includes at least one drawing roll for drawing and pulling the resin fiber tow. The fiber is positioned below the liquid medium liquid level of the oil bath groove, the temperature of the liquid medium in the oil bath groove is above 90 ℃, and the oil bath groove is provided with an inlet and an outlet of the liquid medium and corresponding valves. The arrangement of the inlet and outlet is the same as in the first aspect of the invention.
During the drawing of the fibers, if the temperature of the liquid medium in the oil bath is lowered, the adjustment can be made by flowing in the high-temperature liquid medium and flowing out the low-temperature liquid medium. The low-temperature liquid medium flows into the low-temperature tank through a valve and a pipeline, the temperature of the low-temperature tank is maintained at 20-80 ℃, and the medium does not need to be directly heated to more than 90 ℃ in the low-temperature tank again like the prior art.
In some preferred embodiments, an oil bath storage tank is added on the upper part of the oil bath tank, during the production process, the liquid medium in the low-temperature tank can be preheated to 20-80 ℃ or 20-60 ℃ or 20-50 ℃ or 20-40 ℃ (lower than the temperature of the liquid medium required in the oil bath tank) and conveyed to the oil bath storage tank by a pump, then the oil bath storage tank is heated to above 90 ℃, and then the oil bath tank is introduced, and the reflux part of the liquid medium can be controlled by a valve to reflux to the low-temperature tank for internal circulation, so that the cyclic use is realized.
Through the use of the device, high-temperature liquid can be prevented from being directly pumped by a pump, cavitation can be greatly reduced, the temperature can be conveniently and accurately controlled and the energy consumption can be reduced because the high-temperature heating is carried out in the oil bath storage tank, and the detection shows that the device can control the temperature of the oil bath within +/-1 ℃ during drafting. By using the circulation, the temperature of the fiber tows can be well controlled, and broken filaments or broken filaments are reduced in the drafting process.
Examples
The present invention will be described in more detail with reference to examples, but the present invention is not limited to these examples.
The volume of the oil bath was set to 300L and the solvent used was set to water.
In the control group, the liquid medium (mixture of water and finishing agent) was added to the lower tank in the manner shown in FIG. 1, and directly heated, and after the temperature of the liquid medium in the lower tank reached 98 ℃, the liquid medium was pumped into the oil bath tank through a water pump having a maximum flow rate of 16m3The power is 4Kw, and the temperature of the liquid medium in the oil bath is maintained stable through circulation.
In the experimental group, in the manner shown in fig. 2, the temperature of the liquid medium in the low-temperature tank (same as the composition of the liquid medium in the control group) was controlled to 70 ℃, the temperature of the liquid medium in the oil bath storage tank was controlled to 98 ℃, the water pump used from the low-temperature tank to the oil bath storage tank was identical to the control group, and the oil bath storage tank directly drained the liquid medium to the oil bath tank by valve control, and the temperature was maintained stable by circulation as well.
The target temperature of the oil bath was set to 95 ℃, and the time for filling the oil bath with the liquid medium by the different methods and the fluctuation of the temperature of the liquid medium after filling were counted, and the results are shown in the following table.
| Control group | Experimental group | |
| Fill time | 2min | 40s |
| Temperature fluctuation (. degree. C./h) | 2.58 | 0.87 |
It can be found that by introducing the oil bath storage tank, the time for filling the oil bath with the liquid level can be greatly shortened, which accelerates the operation speed during start and stop; in addition, during normal production, the temperature fluctuation is greatly reduced compared with that of a control group, and the method has great benefits for improving the stability of the whole spinning process and the quality of fibers.
Industrial applicability
The technical scheme of the invention can be industrially used for the production of polyarylene sulfide fibers.
Claims (15)
1. A method of spinning a resin, comprising:
the fibers formed by the resin or the combination thereof are introduced into the liquid medium of the oil bath,
drawing the fibers in the liquid medium,
the liquid medium flows into the oil bath from the oil bath storage tank, the liquid medium flowing out of the oil bath flows into the low-temperature tank, the liquid medium is conveyed into the oil bath storage tank from the low-temperature tank through the conveying pump,
the temperature of the liquid medium in the oil bath storage tank is higher than that of the liquid medium in the low-temperature tank.
2. The method according to claim 1, wherein the glass transition temperature of the resin is 85 ℃ or higher.
3. The method of claim 1 or 2, wherein the resin is a polyarylene sulfide resin.
4. The method according to claim 1 or 2, characterized in that the liquid medium is heated in the oil bath reservoir.
5. The method according to claim 1 or 2, characterized in that the liquid medium is heated above 90 ℃ in the oil bath reservoir.
6. The process according to claim 1 or 2, wherein the temperature of the liquid medium in the oil bath is 90 ℃ or higher.
7. The method according to claim 1 or 2, wherein the temperature of the liquid medium in the low-temperature tank is 20 to 80 ℃.
8. The method according to claim 1 or 2, wherein the temperature of the liquid medium in the low-temperature tank is 60 to 80 ℃.
9. An oil bath for spinning resin, comprising:
an oil bath groove is formed in the bottom of the tank body,
the oil bath storage tank is arranged in the oil bath tank,
a low-temperature groove is arranged on the upper surface of the shell,
the oil bath groove, the oil bath storage tank and the low-temperature groove are connected with a valve through pipelines,
the liquid medium flowing out of the oil bath flows into the low-temperature tank,
the apparatus further comprises a transfer pump to transfer the liquid medium, which is sent from the cryogenic tank into the oil bath storage tank by the transfer pump.
10. The device of claim 9, wherein the glass transition temperature of the resin is 85 ℃ or higher.
11. The device of claim 9 or 10, wherein the resin is a polyarylene sulfide resin.
12. The apparatus according to claim 9 or 10, wherein the oil bath reservoir has a heating means to heat the liquid medium, which is heated in the oil bath reservoir by the heating means.
13. The apparatus according to claim 12, wherein the liquid medium is heated in the oil bath reservoir to above 90 ℃ by a heating means.
14. The apparatus according to claim 9 or 10, wherein a drawing roller is further provided in the oil bath.
15. An apparatus according to claim 9 or 10, wherein the liquid medium flows from the oil bath reservoir into the oil bath.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910156589.7A CN109881271B (en) | 2019-03-01 | 2019-03-01 | Method and device for spinning |
| PCT/CN2019/110820 WO2020177322A1 (en) | 2019-03-01 | 2019-10-12 | Spinning method and apparatus |
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| CN201910156589.7A CN109881271B (en) | 2019-03-01 | 2019-03-01 | Method and device for spinning |
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| CN109881271B true CN109881271B (en) | 2021-02-19 |
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| CN109881271B (en) * | 2019-03-01 | 2021-02-19 | 绍兴裕辰新材料有限公司 | Method and device for spinning |
| CN112921422B (en) * | 2021-01-20 | 2022-08-30 | 中国纺织科学研究院有限公司 | Hot box for drawing yarns |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| NL125156C (en) * | 1960-06-01 | |||
| CA1337498C (en) * | 1989-09-01 | 1995-11-07 | Ephraim Broyer | Thermal treatment of thermoplastic filaments |
| JP2776017B2 (en) * | 1990-08-20 | 1998-07-16 | 東レ株式会社 | Polyphenylene sulfide fiber and method for producing the same |
| KR101849796B1 (en) * | 2010-09-21 | 2018-04-17 | 가부시키가이샤 고센 | Super-high-molecular-weight polyolefin yarn, method for producing same, and drawing device |
| CN201883190U (en) * | 2010-11-10 | 2011-06-29 | 肇庆俊富纤网材料有限公司 | Oil recycling system |
| CN102011202B (en) * | 2010-12-03 | 2015-11-18 | 西安航科等离子体科技有限公司 | Fiber beam spinning washes with water and hot gas spring device |
| CN202380141U (en) * | 2011-12-16 | 2012-08-15 | 杭州贝斯特化纤有限公司 | Drawing bath-heating system |
| CN203295671U (en) * | 2013-06-19 | 2013-11-20 | 宜宾丝丽雅股份有限公司 | Water supplementing supply device for plasticizing tank |
| CN103726113A (en) * | 2013-12-25 | 2014-04-16 | 中国科学院化学研究所 | Novel fiber-drawing hot bath medium and application thereof |
| CN206232857U (en) * | 2016-11-25 | 2017-06-09 | 中复神鹰碳纤维有限责任公司 | The water for improving temperature uniformity in groove leads groove |
| CN106757434B (en) * | 2016-12-02 | 2019-11-05 | 宁波大发化纤有限公司 | A kind of oil bath strand tensile device |
| CN109881271B (en) * | 2019-03-01 | 2021-02-19 | 绍兴裕辰新材料有限公司 | Method and device for spinning |
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