CN112708945B - Coagulation bath for wet spinning and coagulation forming method of polyacrylonitrile spinning solution - Google Patents
Coagulation bath for wet spinning and coagulation forming method of polyacrylonitrile spinning solution Download PDFInfo
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- CN112708945B CN112708945B CN201911015711.5A CN201911015711A CN112708945B CN 112708945 B CN112708945 B CN 112708945B CN 201911015711 A CN201911015711 A CN 201911015711A CN 112708945 B CN112708945 B CN 112708945B
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- fairing
- spinneret
- guide roller
- bath
- gooseneck
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- 230000015271 coagulation Effects 0.000 title claims abstract description 57
- 238000005345 coagulation Methods 0.000 title claims abstract description 57
- 238000009987 spinning Methods 0.000 title claims abstract description 36
- 229920002239 polyacrylonitrile Polymers 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000002166 wet spinning Methods 0.000 title claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 34
- 230000001112 coagulating effect Effects 0.000 claims abstract description 26
- 244000261422 Lysimachia clethroides Species 0.000 claims abstract description 20
- 238000007711 solidification Methods 0.000 claims abstract description 14
- 230000008023 solidification Effects 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 238000002788 crimping Methods 0.000 claims description 15
- 238000007493 shaping process Methods 0.000 claims description 2
- 229920000049 Carbon (fiber) Polymers 0.000 abstract description 11
- 239000004917 carbon fiber Substances 0.000 abstract description 11
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000004804 winding Methods 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 description 38
- 238000001035 drying Methods 0.000 description 7
- 238000009730 filament winding Methods 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012784 inorganic fiber Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 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
- 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
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D13/00—Complete machines for producing artificial threads
- D01D13/02—Elements of machines in combination
-
- 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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical 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)
- Inorganic Fibers (AREA)
Abstract
The invention relates to a coagulating bath for wet spinning and a coagulating forming method of polyacrylonitrile spinning solution, which mainly solve the problems of more guide roller windings and more broken yarns in an overflow groove in the coagulating bath in the prior art. By employing a coagulation bath for wet spinning, comprising: the device comprises a gooseneck, a rectifying plate, a spinneret, a rectifying cover A, a guide roller, a rectifying cover B, an overflow plate and a main body groove body; the rectifying plate is arranged at the left side in the main body groove body; the overflow plate is arranged on the right side in the main body groove body; the gooseneck is arranged at the left end of the main body groove body, one end of the gooseneck, which is connected with the spinning nozzle, is positioned at the right side of the rectifying plate, and the spinning nozzle is covered with a rectifying cover A provided with a wire running channel; the fairing B is arranged on the right side of the main body groove body and can be partially positioned above the solidification liquid level, and the technical scheme that the fairing B is provided with the yarn feeding channel solves the problem well and can be used in the wet spinning production of polyacrylonitrile-based carbon fiber precursor.
Description
Technical Field
The invention relates to wet spinning equipment for producing polyacrylonitrile precursor for carbon fiber, in particular to a coagulation bath for realizing a coagulation process, and particularly relates to a coagulation bath for wet spinning and a coagulation forming method of a polyacrylonitrile spinning solution.
Background
PAN-based carbon fiber is an artificially synthesized inorganic fiber. The fibrous polymer is prepared from acrylonitrile and comonomer through a series of processes of polymerization, spinning, pre-oxidation, carbonization and the like. PAN molecules are mainly physically changed in the spinning process to form white fibrous precursor, and in the pre-oxidation process, the PAN precursor gradually develops into a certain heat-resistant oxygen-containing structure, and carbon fibers with extremely high carbon content are obtained after carbonization. The carbon fiber has the performances of high specific strength, high specific modulus, high temperature resistance, chemical corrosion resistance and the like, so that the application field of the carbon fiber is wide.
High quality PAN precursor is a first requisite for manufacturing high performance carbon fiber, and is one of the most critical factors affecting the quality of carbon fiber. The production of high quality PAN filaments places very high demands on the spinning equipment and process, especially on the process parameters. In the spinning process, the coagulation process is an important process for forming a fiber structure, and the structure of the nascent fiber generated under different coagulation conditions is different. The PAN solution wet spinning solidification forming process is a key step of generating micropores in the fiber, so that the spinning solidification condition plays a decisive role in the performance of the carbon fiber. In addition to micropores, an unreasonable coagulation process during spinning is also one of the key factors that lead to non-uniformity of the as-spun fibers. The coagulation process parameters of wet spinning comprise coagulation bath temperature, concentration, negative draft and the like.
In the process of producing PAN precursor by traditional wet spinning, the coagulation bath mainly comprises a main body tank body, a distribution plate and an overflow plate. When the solidification process is unreasonable, the freshly formed nascent fiber is caused to break under the disturbance action of a solidification liquid flow field; the freshly formed as-formed fibers are subject to tension in the coagulation bath and are subject to stretch action, and yarn breakage is also liable to occur; after the coagulated fiber leaves the coagulation bath, the fiber enters the air atmosphere from the liquid environment, and the coagulated yarn is easily broken due to the combined action of the temperature difference and the tension. These different causes cause the coagulated filaments to be partially or completely broken. The partially broken yarn is wound around the guide roller, and the completely broken yarn is carried to the overflow port of the coagulation liquid along with the flow of the coagulation liquid, so that a lot of broken yarn is collected after accumulation for a certain time in the overflow port of the coagulation bath. Yarn breakage is an important defect of nascent fibers, and is inherited, so that the number of broken filaments is increased, the breakage rate is increased, and the CV value is increased.
A coagulating bath for wet spinning, which introduces a fairing to reduce the influence of flow field and temperature difference on yarn breakage; the adjustment of the guide roller in the height direction and the active and passive power adjustment are increased, and the influence of a tension field on broken wires is overcome; eliminating the phenomena of filament winding of a guide roller in the coagulating bath and excessive filament breakage in the overflow groove.
The patent CN201410430911.8 describes a wet spinning coagulation bath, relates to synthetic fiber wet spinning coagulation forming equipment, and particularly relates to a wet spinning coagulation bath for Polyacrylonitrile (PAN) -based carbon fiber precursor, which comprises three parts, namely a bath liquid inlet buffer area, a channel area and a bath liquid outlet collecting area, according to the traveling direction of a filament bundle, and is characterized in that: the invention has the beneficial effects that the concentration difference of the upper layer and the lower layer of bath liquid can be effectively reduced, the uniform formation of each part of the filament bundle is realized, and the dispersion among filament bundles is reduced.
Disclosure of Invention
One of the technical problems to be solved by the invention is that the guiding roller in the coagulating bath is wound and the overflow groove is broken more in the prior art. There is provided a coagulation bath for wet spinning having a cowling introduced to reduce the influence of a flow field and a temperature difference on yarn breakage; the adjustment of the guide roller in the height direction and the active and passive power adjustment are increased, and the influence of a tension field on broken wires is overcome; eliminating the phenomena of filament winding of a guide roller in the coagulating bath and excessive filament breakage in the overflow groove.
The second technical problem to be solved by the invention is to provide a method for solidifying and forming the polyacrylonitrile spinning solution, and the solidifying bath tank for wet spinning is adopted to solve one of the technical problems.
The third technical problem to be solved by the invention is to provide a preparation method of polyacrylonitrile precursor, which adopts the coagulation bath for wet spinning to carry out coagulation forming, wherein one of the technical problems is solved.
In order to solve one of the technical problems, the technical scheme adopted by the invention is as follows: a coagulating bath for wet spinning, which comprises a gooseneck 3, a rectifying plate 4, a spinneret 5, a rectifying cover A6, a guide roller 7, a rectifying cover B8, an overflow plate 9 and a main body groove 11; wherein, the rectifying plate 4 is arranged at the left side in the main body groove 11; the overflow plate 9 is arranged on the right side in the main body groove body 11; the gooseneck 3 is arranged at the left end of the main body groove body, one end of the gooseneck, which is connected with the spinneret 5, is positioned at the right side of the rectifying plate 4, and the spinneret is covered with a rectifying cover A6 provided with a wire running channel; the fairing B8 is arranged on the right side of the main body groove 11 and can be partially positioned above the solidification liquid level, a wire running channel is arranged in the fairing B, and the guide roller 7 is used for guiding wires to enter the wire running channel in the fairing B or guiding wires entering the fairing B to leave the fairing B.
In the above technical solutions, the "left side" and the "right side" are based on the descriptions shown in fig. 1 and fig. 2 of the present invention, or the directions along the wire running direction are from left to right, and should not be construed as absolute limitations of the present invention.
In the above technical scheme, the fairing A6 is preferably in an axisymmetric structure, one end of the fairing is in airtight connection with the gooseneck 3 connected with the spinneret or the spinneret, and the other end of the fairing is opened for filament discharge; further preferred is: the cross section shape of the fairing A6 is the same as the cross section of the spinneret, and the symmetry axis is parallel to the filament outlet direction.
In the above technical scheme, the wall surfaces around the fairing A6 are preferably provided with small holes for liquid diffusion.
In the above technical solution, the gooseneck may be suspended and fixed or supported and fixed, and further preferably: the coagulation bath also preferably comprises a rotary shaft 1 and a bolt 2; the gooseneck 3 is movably fixed by the rotary shaft 1 and is supported by the bolts 2 arranged on the main body groove body.
In the above technical solution, the rotation angle of the gooseneck 3 around the rotation axis 1 in the vertical plane is preferably less than 180 °; further preferably 0 to 120 °, more preferably more than 0 °.
In the above technical solution, the height of the gooseneck 3 is preferably adjustable by the bolts 2, and the height of the gooseneck 3 is mainly used for adjusting the height of the spinneret 4 and the direction of spinning.
In the above-mentioned technical solution, the included angle between the filament outlet direction of the spinneret 4 and the horizontal direction is preferably adjusted within a range of 0 ° to 10 °, more preferably within a range of 0 ° to 5 °, and even more preferably greater than 0 ° by the bolt 2 and the rotary shaft 1.
In the above technical solution, the coagulation bath for wet spinning may preferably further include a crimping roller 10 for guiding the running yarn to the next process.
In the above technical solution, the height of the guide roller 7 is preferably adjustable, so that the guide roller 7 can be located completely below the solidification liquid level or partially above the solidification liquid level or completely above the solidification liquid level; further preferred is: when the guide roller 7 is completely below the solidification liquid level or is partially above the solidification liquid level, the guide roller 7 is a driven roller; when the guide roller 7 is completely positioned above the solidification liquid level, the guide roller 7 is a driving roller, and the linear speed of the surface of the guide roller 7 is the same as the linear speed of the surface of the crimping roller; more preferably: the plane where the connecting line between the lower edge of the guide roller 7 and the center of the spinneret is positioned is vertical to the surface of the spinneret.
In the above technical solution, the fairing B8 is preferably hollow and cylindrical, two ends of the fairing are open for wire feeding, and an axial line of the fairing is parallel to a wire feeding direction.
According to the invention, through the special-designed coagulating bath, the coagulating bath is provided with the fairing, so that the influence of a flow field and a temperature difference on yarn breakage is reduced; the adjustment of the guide roller in the height direction and the active and passive power adjustment are increased, and the influence of a tension field on broken wires is overcome; eliminating the phenomena of filament winding of a guide roller in the coagulating bath and excessive filament breakage in the overflow groove.
In order to solve the second technical problem, the invention adopts the following technical scheme: a method for solidifying and shaping the spinning liquid of polyacrylonitrile features that in any one of the above technical solutions, the spinning liquid of polyacrylonitrile is sprayed out from spinneret, and then enters solidifying bath via the channel of fairing A, and after passing through the channel of fairing B, the spinning liquid is led to subsequent procedure by crimping rollers.
In the above-mentioned technical solution, the process conditions and the spinning dope are not particularly limited, and those skilled in the art can use the method according to the wet spinning process, for example, but not limited to, the molecular weight of polyacrylonitrile in the polyacrylonitrile spinning dope is preferably 7 to 15 tens of thousands, and the viscosity of the spinning dope is preferably 40pa·s to 120pa·s.
In order to solve the third technical problem, the technical scheme adopted by the invention is as follows: the preparation method of the polyacrylonitrile precursor comprises the step of solidifying and forming the polyacrylonitrile spinning solution by adopting the solidifying bath for wet spinning according to any one of the technical schemes for solving the technical problems.
In the above technical solution, the method for preparing the polyacrylonitrile precursor is not particularly limited, and those skilled in the art can use the method according to a wet spinning process, for example, but not limited to, the molecular weight of polyacrylonitrile in the polyacrylonitrile spinning solution in the coagulation forming step is preferably 7 to 15 tens of thousands, and the viscosity of the spinning solution is preferably 40pa·s to 120pa·s.
By adopting the technical scheme of the invention, the method is used in the wet spinning process of producing polyacrylonitrile precursor for carbon fiber, can ensure that the influence of a flow field and a temperature difference on broken filaments is reduced, and overcomes the influence of a tension field on broken filaments; eliminates the phenomena of filament winding of a guide roller in the coagulating bath and excessive filament breakage in an overflow groove, and achieves better technical effect.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention;
FIG. 2 is a schematic view of the structure of the present invention (5 of the spinneret up);
FIG. 3 is a schematic diagram of a comparative example employed in the present invention;
in fig. 1, 1 is a rotation axis; 2 is a bolt; 3 is a gooseneck; 4 is a rectifying plate; 5 is a spinneret; 6 is a fairing A;7 is a guide roller; 8 is a fairing B;9 is an overflow plate; 10 is a crimping roller; 11 is a main body groove body.
Further description will be given below by way of specific examples.
Detailed Description
[ example 1 ]
Coagulation bath: using and adjusting bolts, and enabling an included angle between the filament outlet direction of the spinneret and the horizontal direction to be 3 degrees in a two-dimensional plane; raising the nascent fiber by 3 degrees in the horizontal direction, and adjusting the height of the guide roller to enable part of the nascent fiber to be immersed into the coagulating liquid; raising the primary fiber in the coagulating bath for 3 DEG in the horizontal direction; the connection line between the lower edge of the guide roller and the center of the spinneret is kept vertical to the surface of the spinneret all the time in a two-dimensional plane, the guide roller is a passive roller, and a fairing A and a fairing B are used for spinning for 24 hours, no filament is wound on the guide roller and the crimping roller, dropped fibers are collected in a coagulation bath overflow tank, and after solvent removal and drying, the quality of the dropped fibers is 0.2677g.
[ example 2 ]
Coagulation bath: using and adjusting bolts, and enabling an included angle between the filament outlet direction of the spinneret and the horizontal direction to be 5 degrees in a two-dimensional plane; the nascent fiber is lifted by 5 degrees in the horizontal direction, and the height of the guide roller is adjusted to be completely positioned above the liquid level of the coagulating liquid; raising the primary fiber in the coagulating bath for 5 DEG in the horizontal direction; the connection line between the lower edge of the guide roller and the center of the spinneret is kept vertical to the surface of the spinneret all the time in a two-dimensional plane, the guide roller is a driving roller, the linear speed of the surface of the guide roller is the same as that of the surface of the crimping roller, a fairing A and a fairing B are used, after spinning for 24 hours, the upper surfaces of the guide roller and the crimping roller are free from filament winding, the dropped fibers are collected in a coagulation bath overflow tank, and after solvent removal and drying, the filament dropping quality is 0.1557g.
[ example 3 ]
Coagulation bath: using and adjusting bolts, and enabling an included angle between the filament outlet direction of the spinneret and the horizontal direction to be 0 degree in a two-dimensional plane; the direction of the nascent fiber is kept horizontal, and the height of the guide roller is adjusted to enable the nascent fiber to be completely immersed into the coagulating liquid; leveling the direction of the nascent fiber in the coagulation bath; the connection line between the lower edge of the guide roller and the center of the spinneret is kept vertical to the surface of the spinneret all the time in a two-dimensional plane, the guide roller is a passive roller, and a fairing A and a fairing B are used for spinning for 24 hours, no filament is wound on the guide roller and the crimping roller, dropped fibers are collected in a coagulation bath overflow tank, and after solvent removal and drying, the quality of the dropped fibers is 0.3112g.
[ example 4 ]
Coagulation bath: using and adjusting bolts, and enabling an included angle between the filament outlet direction of the spinneret and the horizontal direction to be 4 degrees in a two-dimensional plane; the nascent fiber is lifted by 4 degrees in the horizontal direction, and the height of the guide roller is adjusted to be completely positioned above the coagulating liquid; raising the primary fiber in the coagulating bath for 4 DEG in the horizontal direction; the connection line between the lower edge of the guide roller and the center of the spinneret is kept vertical to the surface of the spinneret all the time in a two-dimensional plane, the guide roller is a driving roller, the linear speed of the surface of the guide roller is the same as that of the surface of the crimping roller, a fairing A and a fairing B are used, after spinning for 24 hours, the upper surfaces of the guide roller and the crimping roller are free from filament winding, the dropped fibers are collected in a coagulation bath overflow tank, and after solvent removal and drying, the filament dropping quality is 0.1733g.
[ example 5 ]
Coagulation bath: using and adjusting bolts, and enabling an included angle between the filament outlet direction of the spinneret and the horizontal direction to be 1 degree in a two-dimensional plane; the nascent fiber is lifted by 1 degree in the horizontal direction, and the height of the guide roller is adjusted to be completely positioned in the coagulating liquid; raising the primary fiber in the coagulating bath by 1 DEG in the horizontal direction; the connection line between the lower edge of the guide roller and the center of the spinneret is kept vertical to the surface of the spinneret all the time in a two-dimensional plane, the guide roller is a passive roller, and a fairing A and a fairing B are used for spinning for 24 hours, no filament is wound on the guide roller and the crimping roller, dropped fibers are collected in a coagulation bath overflow tank, and after solvent removal and drying, the quality of the dropped fibers is 0.1254g.
[ example 6 ]
Coagulation bath: using and adjusting bolts, and enabling an included angle between the filament outlet direction of the spinneret and the horizontal direction to be 2 degrees in a two-dimensional plane; raising the nascent fiber by 2 degrees in the horizontal direction, and adjusting the height of the guide roller to enable part of the nascent fiber to be immersed into the coagulating liquid; raising the primary fiber in the coagulating bath by 2 degrees in the horizontal direction; the connection line between the lower edge of the guide roller and the center of the spinneret is kept vertical to the surface of the spinneret all the time in a two-dimensional plane, the guide roller is a passive roller, and a fairing A and a fairing B are used for spinning for 24 hours, no filament is wound on the guide roller and the crimping roller, dropped fibers are collected in a coagulation bath overflow tank, and after solvent removal and drying, the quality of the dropped fibers is 0.4225g.
[ comparative example 1 ]
Coagulation bath: the schematic structure of the coagulation bath is shown in fig. 3, and the height of the guide roller is adjusted without using an adjusting bolt 2 so that the guide roller is partially immersed in the coagulation liquid; raising the direction of the nascent fiber in the coagulating bath 3 DEG in the horizontal direction; the guide roller is a passive roller, and a fairing A and a fairing B are not used, after spinning for 24 hours, a large number of fiber winding rollers are arranged on the guide roller and the crimping roller, dropped fibers are collected in a coagulation bath overflow tank, and after solvent removal and drying, the dropped fibers have a quality of 3.3578g.
As can be seen from comparative example 1 and example 1, after the coagulation bath of the invention is adopted, the influence of a flow field and a temperature difference on broken wires can be reduced, the influence of a tension field on broken wires is overcome, and the phenomena of filament winding of a filament guiding roller in the coagulation bath and excessive broken wires in an overflow groove are eliminated.
Claims (8)
1. A coagulating bath for wet spinning comprises a gooseneck (3), a rectifying plate (4), a spinneret (5), a rectifying cover A (6), a guide roller (7), a rectifying cover B (8), an overflow plate (9) and a main body groove body (11); wherein the rectifying plate (4) is arranged at the left side in the main body groove body (11); the overflow plate (9) is arranged on the right side in the main body groove body (11); the gooseneck (3) is arranged at the left end of the main body groove body, one end of the gooseneck, which is connected with the spinneret (5), is positioned at the right side of the rectifying plate (4), and the spinneret is covered with a rectifying cover A (6) provided with a wire running channel; the fairing B (8) is arranged on the right side of the main body groove body (11) and can be partially positioned above the solidification liquid level, a wire passage is arranged in the fairing B, a guide roller (7) is used for guiding wires to enter the wire passage in the fairing B or guiding wires entering the fairing B to leave the fairing B, and the lower edge of the guide roller (7) is vertical to the plane where the connecting line of the center of the spinneret is positioned and the surface of the spinneret; wherein, the fairing A (6) is in an axisymmetric structure, one end of the fairing A is in airtight connection with a gooseneck (3) connected with a spinneret, and the other end of the fairing A is opened for filament discharge; the section shape of the fairing A (6) is the same as the section of the spinneret, and the symmetry axis is parallel to the filament outlet direction; the wall surfaces around the fairing A (6) are provided with small holes; the fairing B (8) is hollow and cylindrical, two sides of the fairing B are open for wire feeding, and the axial line of the fairing B is parallel to the wire feeding direction;
the coagulating bath also comprises a rotating shaft (1) and a bolt (2); the gooseneck (3) is movably fixed by the rotating shaft (1) and is supported by the bolts (2) arranged on the groove body of the main body; the included angle between the filament outlet direction of the spinneret (4) and the horizontal direction is adjusted within the range of 0-5 degrees and more than 0 degrees through the bolt (2) and the rotary shaft (1).
2. Coagulation bath for wet spinning according to claim 1, characterized in that the rotation angle of the gooseneck (3) about the rotation axis (1) in the vertical plane is less than 180 °.
3. Coagulation bath for wet spinning according to claim 1, characterized in that the height of the gooseneck (3) is adjustable by means of bolts (2).
4. Coagulation bath for wet spinning according to claim 1, characterized in that the height of the guide rolls (7) is adjustable such that the guide rolls (7) can be located completely below the coagulation liquid level or partially above the coagulation liquid level or completely above the coagulation liquid level.
5. Coagulation bath for wet spinning according to claim 4, characterized in that the guiding roll (7) is a passive roll when the guiding roll (7) is completely below the coagulation liquid level or partly above the coagulation liquid level; when the guide roller (7) is completely positioned above the solidification liquid level, the guide roller (7) is a driving roller, and the linear speed of the surface of the guide roller (7) is the same as the linear speed of the surface of the crimping roller.
6. A method for solidifying and forming a polyacrylonitrile spinning solution, which adopts the solidifying bath tank for wet spinning according to any one of claims 1-5, wherein the polyacrylonitrile spinning solution is sprayed out from a spinneret, enters the solidifying bath through a wire-moving channel of a fairing A, and is guided to a subsequent process by a crimping roller after passing through a wire-moving channel in a fairing B.
7. The method for solidifying and shaping a polyacrylonitrile spinning solution according to claim 6, wherein the molecular weight of polyacrylonitrile in the polyacrylonitrile spinning solution is 7 ten thousand to 15 ten thousand, and the viscosity of the spinning solution is 40 pa.s to 120 pa.s.
8. A method for preparing polyacrylonitrile precursor, which comprises the step of solidifying and forming the polyacrylonitrile spinning solution by adopting the solidifying bath for wet spinning according to any one of claims 1-5.
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| CN201911015711.5A CN112708945B (en) | 2019-10-24 | 2019-10-24 | Coagulation bath for wet spinning and coagulation forming method of polyacrylonitrile spinning solution |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07207522A (en) * | 1994-01-11 | 1995-08-08 | Toray Ind Inc | Spinning method of acrylonitrile type fiber and its apparatus |
| JPH10183420A (en) * | 1996-12-18 | 1998-07-14 | Japan Exlan Co Ltd | Horizontal wet-coagulation bath and wet-spinning using the coagulation bath |
| JPH11229227A (en) * | 1998-02-13 | 1999-08-24 | Kanegafuchi Chem Ind Co Ltd | Straightening device for wet spinning |
| JP2004270067A (en) * | 2003-03-07 | 2004-09-30 | Teijin Ltd | Dry-wet spinning apparatus |
| CN201908162U (en) * | 2010-12-17 | 2011-07-27 | 东华大学 | Device for preparing nanofiber continuous filament yarn |
| CN104213209A (en) * | 2014-08-25 | 2014-12-17 | 朱自平 | Wet-spinning coagulating bath |
-
2019
- 2019-10-24 CN CN201911015711.5A patent/CN112708945B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07207522A (en) * | 1994-01-11 | 1995-08-08 | Toray Ind Inc | Spinning method of acrylonitrile type fiber and its apparatus |
| JPH10183420A (en) * | 1996-12-18 | 1998-07-14 | Japan Exlan Co Ltd | Horizontal wet-coagulation bath and wet-spinning using the coagulation bath |
| JPH11229227A (en) * | 1998-02-13 | 1999-08-24 | Kanegafuchi Chem Ind Co Ltd | Straightening device for wet spinning |
| JP2004270067A (en) * | 2003-03-07 | 2004-09-30 | Teijin Ltd | Dry-wet spinning apparatus |
| CN201908162U (en) * | 2010-12-17 | 2011-07-27 | 东华大学 | Device for preparing nanofiber continuous filament yarn |
| CN104213209A (en) * | 2014-08-25 | 2014-12-17 | 朱自平 | Wet-spinning coagulating bath |
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| CN112708945A (en) | 2021-04-27 |
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