CN111893668A - Homogenization treatment device and method, and preparation method of polyacrylonitrile-based carbon fiber - Google Patents
Homogenization treatment device and method, and preparation method of polyacrylonitrile-based carbon fiber Download PDFInfo
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- CN111893668A CN111893668A CN202010646779.XA CN202010646779A CN111893668A CN 111893668 A CN111893668 A CN 111893668A CN 202010646779 A CN202010646779 A CN 202010646779A CN 111893668 A CN111893668 A CN 111893668A
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- 229920002239 polyacrylonitrile Polymers 0.000 title claims abstract description 213
- 238000000265 homogenisation Methods 0.000 title claims abstract description 42
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 38
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims description 28
- 239000000835 fiber Substances 0.000 claims abstract description 197
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 87
- 238000005507 spraying Methods 0.000 claims abstract description 79
- 238000001035 drying Methods 0.000 claims abstract description 70
- 230000005540 biological transmission Effects 0.000 claims abstract description 32
- 230000009471 action Effects 0.000 claims abstract description 24
- 238000007254 oxidation reaction Methods 0.000 claims description 23
- 230000003647 oxidation Effects 0.000 claims description 21
- 239000007921 spray Substances 0.000 claims description 10
- 230000007246 mechanism Effects 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 6
- 239000002699 waste material Substances 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 10
- 239000002243 precursor Substances 0.000 description 17
- 230000000694 effects Effects 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 238000006073 displacement reaction Methods 0.000 description 4
- 238000007363 ring formation reaction Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
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- 230000001174 ascending effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B1/00—Applying liquids, gases or vapours onto textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing or impregnating
- D06B1/02—Applying liquids, gases or vapours onto textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing or impregnating by spraying or projecting
-
- 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
-
- 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
- D01F9/32—Apparatus therefor
- D01F9/328—Apparatus therefor for manufacturing filaments from polyaddition, polycondensation, or polymerisation products
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B15/00—Removing liquids, gases or vapours from textile materials in association with treatment of the materials by liquids, gases or vapours
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B23/00—Component parts, details, or accessories of apparatus or machines, specially adapted for the treating of textile materials, not restricted to a particular kind of apparatus, provided for in groups D06B1/00 - D06B21/00
- D06B23/20—Arrangements of apparatus for treating processing-liquids, -gases or -vapours, e.g. purification, filtration or distillation
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Abstract
The invention relates to a homogenizing device and a homogenizing method and a preparation method of polyacrylonitrile-based carbon fibers, and relates to the technical field of carbon fibers. The main technical scheme adopted is as follows: a homogenizing device is used for homogenizing polyacrylonitrile fibers before a step of pre-oxidizing the polyacrylonitrile fibers, wherein the homogenizing device comprises a spraying device and a drying and preheating device. The spraying device is used for spraying water on the surface of the polyacrylonitrile fiber. The drying and preheating device is used for drying and preheating the polyacrylonitrile fiber after spraying treatment, and the polyacrylonitrile fiber is enabled to keep the set water content. Under the traction action of the transmission device, the polyacrylonitrile fiber is firstly sprayed by the spraying device and then dried and preheated by the drying and preheating device. The invention mainly reduces the water content discrete coefficient of the polyacrylonitrile fiber by controlling the water content of the polyacrylonitrile fiber, and carries out continuous homogenization treatment on the polyacrylonitrile fiber.
Description
Technical Field
The invention relates to the technical field of carbon fibers, in particular to a homogenization treatment device and method and a preparation method of polyacrylonitrile-based carbon fibers.
Background
The polyacrylonitrile-based carbon fiber is an inorganic polymer fiber with carbon content higher than 90%. The wind power generation device is widely applied to the fields of aerospace, rail transit, wind power generation, sports equipment and the like. The preparation process of the polyacrylonitrile-based carbon fiber comprises the following steps: the polyacrylonitrile fiber (the polyacrylonitrile fiber refers to a precursor of polyacrylonitrile-based carbon fiber, and is also called as "precursor") is prepared, and the operations of pre-oxidation, carbonization, surface treatment, sizing and the like are sequentially performed on the polyacrylonitrile fiber to obtain the polyacrylonitrile-based carbon fiber.
At present, the main process flow of the preoxidation process of polyacrylonitrile fibers is as follows: the polyacrylonitrile fiber is directly sent into an oxidation furnace for pre-oxidation through a transmission roller under the tension control of a yarn withdrawing creel. In the prior art, a preheating step is additionally arranged between a step of fiber withdrawing of polyacrylonitrile fibers and a step of preoxidation of the polyacrylonitrile fibers so as to dehydrate and deoil the polyacrylonitrile fibers and reduce the pollution of water and oil to a preoxidation furnace.
However, the inventors of the present invention found that the existing preparation process of polyacrylonitrile-based carbon fiber has at least the following problems: before the polyacrylonitrile fiber enters the oxidizing furnace, the difference of the water content of the polyacrylonitrile fiber at different stations is large, so that the cyclization reaction degree of the polyacrylonitrile fiber at different stations is inconsistent in the pre-oxidation process, and the dispersion coefficient deviation of the mechanical property of the polyacrylonitrile-based carbon fiber at different stations is large. Meanwhile, the continuous homogenization treatment of the polyacrylonitrile fiber in the prior art is less researched.
Disclosure of Invention
In view of the above, the present invention provides a homogenization apparatus and a method thereof, and a method for preparing polyacrylonitrile-based carbon fibers, and the main objective thereof is: before the polyacrylonitrile fiber is subjected to pre-oxidation treatment, the water content discrete coefficients of the polyacrylonitrile fiber at different stations can be reduced.
It should be noted that the term "polyacrylonitrile fiber" in the present invention refers to a precursor of polyacrylonitrile-based carbon fiber, and is colloquially referred to as "precursor fiber" by those skilled in the art.
In order to achieve the purpose, the invention mainly provides the following technical scheme:
in one aspect, an embodiment of the present invention provides a homogenization treatment apparatus for performing homogenization treatment on polyacrylonitrile fibers after a step of filament withdrawing of the polyacrylonitrile fibers and before a step of pre-oxidation of the polyacrylonitrile fibers, wherein the homogenization treatment apparatus includes:
the spraying device is used for spraying water on the surface of the polyacrylonitrile fibers;
the drying and preheating device is used for drying and preheating the polyacrylonitrile fibers subjected to spraying treatment and keeping the polyacrylonitrile fibers at a set water content;
under the traction action of the transmission device, the polyacrylonitrile fiber is firstly sprayed by the spraying device and then dried and preheated by the drying and preheating device.
Preferably, the homogenization treatment apparatus further comprises:
the tension balancing device is used for adjusting the tension of the polyacrylonitrile fiber and adjusting the tension value of the polyacrylonitrile fiber to a target tension value;
the polyacrylonitrile fiber sequentially passes through the spraying device, the tension balancing device and the drying and preheating device under the traction action of the transmission device; or
The polyacrylonitrile fiber passes through the tension balancing device, the spraying device and the drying and preheating device in sequence under the traction action of the transmission device.
Preferably, the spraying device comprises a spraying pipeline and a spraying head; the spraying head is connected with the spraying pipeline and is used for spraying water on the surface of the polyacrylonitrile fiber passing through the spraying device; preferably, the spraying device further comprises a water tank; wherein the water tank is positioned below the spray header; and the polyacrylonitrile fiber passes through the spraying device between the spraying head and the water tank under the traction action of the transmission device.
Preferably, the drying preheating means includes a plurality of drying heat rollers; the polyacrylonitrile fiber sequentially passes through a plurality of drying hot rollers in the drying and preheating device under the traction action of the transmission device; preferably, the homogenizing device further comprises a waste discharge cover for discharging water vapor generated during drying and preheating of the polyacrylonitrile fibers to the outside; preferably, the temperature of the drying thermo roll is adjusted in the range of 50 to 200 ℃.
Preferably, the tension balancing means includes: the tension adjusting device comprises a first guide roller, a tension adjusting roller, a second guide roller and an adjusting device; wherein,
the polyacrylonitrile fiber passes through a first guide roller, a tension adjusting roller and a second guide roller in sequence under the traction action of a transmission device; the polyacrylonitrile fiber which horizontally runs downwards longitudinally after being guided by the first guide roller; the polyacrylonitrile fiber which runs longitudinally downwards runs longitudinally upwards after being guided by the tension adjusting roller; the polyacrylonitrile fiber which runs longitudinally and upwards runs horizontally after being guided by the second guide roller;
the adjusting device is used for adjusting the position of the tension adjusting roller in the longitudinal direction so as to adjust the tension of the polyacrylonitrile fibers;
preferably, the tension adjusting range of the tension balancing device is 50-2000 cN.
Preferably, the adjusting device comprises a transmission belt, a water tank and a heavy object; wherein the weight is disposed in the water tank; one end of the transmission belt is connected with the tension adjusting roller, the transmission belt extends upwards, and the other end of the transmission belt is connected with the heavy object after being guided by the guide structure; the position of the weight when the stress is balanced is adjusted by adjusting the water storage capacity in the water tank, and the position of the tension adjusting roller in the longitudinal direction is further adjusted; or
The adjusting device comprises a driving mechanism, wherein the driving mechanism is connected with the tension adjusting roller and is used for adjusting the position of the tension adjusting roller in the longitudinal direction by driving the tension adjusting roller to move up or down; preferably, the drive mechanism comprises a pneumatic cylinder.
In another aspect, an embodiment of the present invention provides a homogenization method, where the homogenization method is used to homogenize polyacrylonitrile fibers after a step of fiber unwinding and before a step of pre-oxidizing the polyacrylonitrile fibers, where the homogenization method includes the following steps:
water spraying: carrying out water spraying treatment on polyacrylonitrile fibers so as to enable the surfaces of the polyacrylonitrile fibers to be attached with water;
drying and preheating: and drying and preheating the polyacrylonitrile fiber after the spraying treatment so as to dry the polyacrylonitrile fiber and keep the polyacrylonitrile fiber at a set water content.
Preferably, the step of homogenizing further comprises:
and (3) tension balance: performing tension adjustment on the polyacrylonitrile fiber to adjust the tension of the polyacrylonitrile fiber to a target value;
wherein the step of tension balancing is performed after the step of water spraying and before the step of drying and preheating; or the step of tension balancing is performed before the step of water spraying.
Preferably, the polyacrylonitrile fibers are homogenized by the homogenizing device according to any one of the above-mentioned homogenizing devices.
Preferably, when the homogenizing apparatus includes a tension balancing device, and the tension balancing device includes a first guide roller, a tension adjusting roller, a second guide roller, and an adjusting device:
if the tension value of the polyacrylonitrile fiber is smaller than the target tension value, enabling the tension adjusting roller to longitudinally move downwards by a first set distance through the adjusting device when the polyacrylonitrile fiber passes through the tension balancing device;
and if the tension value of the polyacrylonitrile fiber is greater than the target tension value, enabling the tension adjusting roller to longitudinally rise for a second set distance through the adjusting device when the polyacrylonitrile fiber passes through the tension balancing device.
In another aspect, an embodiment of the present invention provides a method for preparing polyacrylonitrile-based carbon fibers, which further includes, after a step of filament withdrawing of polyacrylonitrile fibers and before a step of pre-oxidizing of polyacrylonitrile fibers in a process of preparing polyacrylonitrile-based carbon fibers: homogenizing polyacrylonitrile fibers; wherein,
homogenizing polyacrylonitrile fibers by using the homogenizing device; and/or
The polyacrylonitrile fiber is homogenized by adopting the homogenization method.
Compared with the prior art, the homogenization treatment device and the method and the preparation method of the polyacrylonitrile-based carbon fiber have the following beneficial effects:
on one hand, the homogenization treatment device and the homogenization treatment method provided by the embodiment of the invention can uniformly adhere a certain amount of water to the surface of the polyacrylonitrile fiber through the spraying device, so that broken filaments generated by the electrostatic action of the fiber can be reduced. And then, drying the polyacrylonitrile fiber by a drying and preheating device, and simultaneously controlling the polyacrylonitrile fiber to keep a certain water content so as to homogenize the water content of the polyacrylonitrile fiber.
Furthermore, according to the homogenization treatment device and method provided by the embodiment of the invention, the tension of the polyacrylonitrile fibers is adjusted through the tension balancing device, so that the tensions of the polyacrylonitrile fibers at different stations are kept consistent, and finally, under the action of the drying hot roller, the water-containing homogenization effect is performed on the precursor, so that the performance of the polyacrylonitrile fibers before entering the oxidation furnace is kept consistent, and the problem that the dispersion coefficient of the performance index of the polyacrylonitrile-based carbon fibers is larger is solved.
On the other hand, the polyacrylonitrile-based carbon fiber provided by the embodiment of the invention is additionally provided with the step of homogenizing the polyacrylonitrile fiber after the step of removing the polyacrylonitrile fiber and before the step of pre-oxidizing the polyacrylonitrile fiber in the preparation process of the polyacrylonitrile-based carbon fiber, so that the performance dispersion coefficient of the prepared polyacrylonitrile-based carbon fiber is more uniform. Therefore, the invention meets the expected design target requirement and improves the economic benefit.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is a schematic diagram of a homogenizing apparatus according to an embodiment of the present invention;
fig. 2 is a schematic flow chart of a homogenization treatment method according to an embodiment of the present invention.
Detailed Description
To further explain the technical means and effects of the present invention adopted to achieve the predetermined object, the following detailed description of the embodiments, structures, features and effects according to the present invention will be made with reference to the accompanying drawings and preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
Example 1
In one aspect, the present embodiment provides a homogenization apparatus for homogenizing polyacrylonitrile fibers after a step of fiber withdrawal and before a step of pre-oxidizing the polyacrylonitrile fibers. As shown in fig. 1, the homogenization treatment apparatus in the present embodiment includes: spray set and dry preheating device. Wherein the spraying device is used for spraying water on the surface of the polyacrylonitrile fiber 1. The drying and preheating device is used for drying and preheating the polyacrylonitrile fiber 1 after spraying treatment, and the polyacrylonitrile fiber 1 is enabled to keep the set water content. Wherein, the polyacrylonitrile fiber 1 is firstly sprayed by a spraying device and then dried and preheated by a drying and preheating device under the traction action of a transmission device.
Preferably, the spray device comprises a spray pipe 21 and a spray header 22; wherein, the spray header 22 is connected with the spray pipeline 21 and is used for spraying water on the surface of the polyacrylonitrile fiber 1 passing through the spray device. Preferably, the spraying device further comprises a water tank 23; wherein, the water tank 23 is positioned below the spray header 22; the polyacrylonitrile fiber 1 passes through the spraying device between the spraying head 22 and the water tank 23 under the traction action of the transmission device.
Preferably, the drying preheating means includes a plurality of drying heat rollers 41; wherein, the polyacrylonitrile fiber 1 passes through a plurality of drying hot rollers 41 in the drying and preheating device in sequence under the traction action of the transmission device. Preferably, the number of the drying heat roller 41 is 8.
Preferably, the homogenizing apparatus further includes a waste hood 42 for exhausting water vapor generated during the drying and preheating of the polyacrylonitrile fibers to the outside. Wherein the temperature adjusting range of the drying hot roller is 50-200 ℃.
In the homogenization apparatus provided in this embodiment, a certain amount of water is uniformly attached to the surface of the polyacrylonitrile fibers by the spraying device, so that the fuzz generated by the electrostatic interaction of the fibers can be reduced. And then, drying the polyacrylonitrile fibers after the temperature of the hot roller is optimally set according to a certain temperature gradient by a drying and preheating device, ensuring that the polyacrylonitrile fibers at different stations keep certain water content, wherein the control range of the water content is generally 0.7-0.9%, and performing water-containing homogenization on the polyacrylonitrile fibers. The optimal temperature setting of the hot rollers according to a certain temperature gradient specifically means that in the drying and preheating device, the temperature of the next hot roller is 10-20 ℃ higher than that of the previous drying hot roller. Wherein the temperature of the starting hot roll is generally 50-70 ℃ and the temperature of the terminating hot roll is 170-200 ℃. After the drying and preheating step, manual sampling and inspection are carried out before the raw materials enter the oxidation furnace.
The polyacrylonitrile fiber is controlled to keep a certain water content, and has the following positive effects: in the initial stage of pre-oxidation, the water in the polyacrylonitrile fiber is combined with the oxygen-containing functional group generated by the reaction of the polyacrylonitrile fiber, so that the mutual entanglement of molecular chains in the fiber structure is strengthened, the reaction capability of part of macromolecular chain segments is frozen, the cyclization reaction rate is relaxed and effectively controlled, the formation of a compact oxide layer structure is reduced, the diffusion and permeation of oxygen molecules in the air are facilitated, meanwhile, micro-pores are generated on the surface of the fiber by water, the oxygen enters and the waste generated by the reaction escapes, the double diffusion effect in the pre-oxidation process is enhanced, the skin-core structure of the pre-oxidized fiber is reduced, and the homogenized fiber can be obtained. Wherein the moisture content is (sampling filament bundle-drying filament bundle)/drying filament bundle x 100%.
If the polyacrylonitrile fiber contains excessive moisture, the reaction rate of the cyclization degree of the polyacrylonitrile fiber is too low. The cyclization degree is the premise of oxidation reaction, the oxidation reaction is lower, the fiber pre-oxidation degree is insufficient, the sheath-core structure of the pre-oxidized fiber is too large, the fiber homogenization degree is reduced, and the performance is reduced.
Therefore, the water content of the polyacrylonitrile fibers with the set amount is controlled, the consistency of the pre-oxidation degrees of the polyacrylonitrile fibers in different stations can be improved, and the homogenization of the polyacrylonitrile-based carbon fibers can be further improved.
Example 2
Preferably, the homogenizing device of this embodiment further includes a tension balancing device for adjusting the tension of the polyacrylonitrile fiber to a target tension value, as shown in fig. 1.
The polyacrylonitrile fiber sequentially passes through the spraying device, the tension balancing device and the drying and preheating device under the traction action of the transmission device; or the polyacrylonitrile fiber passes through the tension balancing device, the spraying device and the drying and preheating device in sequence under the traction action of the transmission device.
Preferably, the tension balancing device in this embodiment includes: a first guide roller 31, a tension adjusting roller 33, a second guide roller 32 and an adjusting device (the first guide roller 31 and the second guide roller 32 are fixed on a bracket and are respectively driven by a motor, and two rolling bearings are arranged at the two ends of the tension adjusting roller 33). Wherein, the polyacrylonitrile fiber passes through a first guide roller 31, a tension adjusting roller 33 and a second guide roller 32 in sequence under the traction action of a transmission device. The polyacrylonitrile fiber which horizontally runs downwards longitudinally after being guided by the first guide roller 31; the polyacrylonitrile fiber which runs longitudinally downwards runs longitudinally upwards after being guided by the tension adjusting roller 33; the polyacrylonitrile fiber running longitudinally upward runs horizontally after being guided by the second guide roller 32. Wherein, the adjusting device is used for adjusting the position of the tension adjusting roller 33 in the longitudinal direction (i.e. the tension adjusting roller 33 is moved upwards or downwards along the longitudinal direction by the adjusting device) so as to adjust the tension of the polyacrylonitrile fiber. Preferably, the tension adjusting range of the tension balancing device is 50-2000 cN.
Further preferably, the adjusting device in the present embodiment is configured as follows:
the adjustment means comprise a belt 34, a water tank 38 and a weight 37. A weight 37 is placed in the water tank 38. One end of the belt 34 is connected to the tension adjusting roller 33, and the belt extends upward (i.e., the end of the belt connected to the tension adjusting roller 33 is a lower end), and the other end of the belt passes through the guide rollers (the third guide roller 35 and the fourth guide roller 36) and is connected to the weight 37. Wherein the position of the weight 37 when the force is balanced is adjusted by adjusting the water storage amount in the water tank 38, thereby adjusting the position of the tension adjusting roller 33 in the longitudinal direction.
For example: (1) the target tension value for the running tow was 2000cN, while the tension value for the tow at the current tension balancing device was 1500 cN. Here, by injecting water into the water tank 38, the buoyancy generated by the weight 37 gradually increases with the rise of the water level, at this time, the tension of the tension adjusting roller applied to the weight plus the buoyancy applied to the weight is greater than the gravity of the weight itself, the weight 38 gradually floats up under the action of the transmission belt 34, the tension adjusting roller 33 sinks down, the draft tension applied to the filament bundle increases, when the balance between the tension adjusting roller 33 and the weight 37 is reestablished, the descending displacement of the tension adjusting roller 37 is h, and the ascending displacement of the weight 37 is h, thereby realizing the adjustment of the tension of the filament bundle. (2) The target tension value for the running tow was 2000cN, while the tension value for the tow at the present tension equalizer was 2500 cN. Through making water tank 38 drainage, along with the reduction of water tank liquid level, the buoyancy that the heavy object 37 produced reduces gradually, and at this moment, the pulling force of the tension adjusting roller that the heavy object receives plus the buoyancy that receives is less than the gravity of heavy object self, and heavy object 37 sinks gradually under the effect of drive belt, and tension adjusting roller 33 then rises, and then the draft tension that the silk bundle bore reduces, and when waiting to reach tension adjusting roller 33 and heavy object 37 and reestablish the balance, the displacement that tension adjusting roller 33 took place to rise is h, and the displacement that the heavy object 37 descends is h, and then realize the regulation to silk bundle tension. Under normal conditions, the tow tension increases by 100cN for every 0.5cm decrease of the dancer 33.
In addition, the adjusting device may be designed as follows in addition to the above structure: the adjusting device comprises a driving mechanism, wherein the driving mechanism is connected with the tension adjusting roller 33, and the position of the tension adjusting roller 33 in the longitudinal direction is adjusted by driving the tension adjusting roller 33 to move up or down. Here, the driving mechanism includes an air cylinder, and the tension adjusting roller 33 is driven to ascend or descend by the air cylinder.
In conclusion, the homogenization treatment device provided by the embodiment adjusts the tension of the polyacrylonitrile fiber through the tension balancing device, so that the tensions of the polyacrylonitrile fiber at different stations are kept consistent, and finally, under the action of the drying hot roller, the water-containing homogenization effect is performed on the precursor, so that the consistency of the performance of the polyacrylonitrile fiber before entering the oxidation furnace is kept, and the problem of large dispersion coefficient of the performance index of the carbon fiber is finally solved.
Preferably, the homogenizing device in the above embodiment further includes a homogenizing chamber, and the spraying device, the tension balancing device, and the drying and preheating device are disposed in the homogenizing chamber. And the homogenizing treatment chamber is provided with a tow inlet and a tow outlet. The polyacrylonitrile fiber tows enter the homogenizing treatment chamber from the tow inlet, are sequentially sprayed, tension balanced and dried and preheated (or tension balanced, sprayed and dried and preheated), and are then drawn out from the tow outlet.
Example 3
On the other hand, this example provides a homogenization method for homogenizing polyacrylonitrile fibers after the step of removing the filaments of the polyacrylonitrile fibers and before the step of pre-oxidizing the polyacrylonitrile fibers, as shown in fig. 2. Wherein, the homogenization treatment method comprises the following steps:
water spraying: and carrying out water spraying treatment on the polyacrylonitrile fiber so as to attach water to the surface of the polyacrylonitrile fiber.
Drying and preheating: and drying and preheating the polyacrylonitrile fiber after the spraying treatment so as to dry the polyacrylonitrile fiber and keep the polyacrylonitrile fiber at a set water content.
Preferably, the step of homogenizing further comprises:
and (3) tension balance: performing tension adjustment on the polyacrylonitrile fiber to adjust the tension of the polyacrylonitrile fiber to a target value; wherein the step of tension balancing is performed after the step of water spraying and before the step of drying and preheating; or the step of tension balancing is performed before the step of water spraying.
In the homogenization treatment method provided by the embodiment, a layer of water is uniformly attached to the surface of the precursor through the spraying step, the tension of the precursor at different stations is kept consistent through the adjustment of the tension balancing device, and finally, under the action of the drying hot roller, the water-containing homogenization effect is performed on the precursor, so that the performance of the precursor before entering the oxidation furnace is kept consistent, and the problem that the coefficient of variation of the performance index of the carbon fiber is large is finally solved.
Preferably, the polyacrylonitrile fibers are homogenized by the homogenizing apparatuses described in examples 1 and 2.
Preferably, as shown in fig. 1, in the tension balancing step:
(1) if the tension value of the polyacrylonitrile fiber is smaller than the target tension value, when the polyacrylonitrile fiber 1 passes through the tension balancing device, the tension adjusting roller 33 is longitudinally moved downwards by a first set distance through the adjusting device.
As shown in fig. 1, water may be added to the water tank 38 to raise the weight 37 a first set distance, and the tension adjusting roller 33 may be moved longitudinally downward a first set distance by the belt 34.
Of course, the tension adjusting roller 33 may be directly driven by the air cylinder to move down by the first set distance in the longitudinal direction.
(2) And if the tension value of the polyacrylonitrile fiber is greater than the target tension value, enabling the tension adjusting roller to longitudinally rise for a second set distance through the adjusting device when the polyacrylonitrile fiber passes through the tension balancing device.
As shown in fig. 1, the water tank 38 may be drained, the weight 37 may be lowered a second set distance, and the tension adjusting roller 33 may be raised longitudinally a second set distance by the belt 34.
Of course, the tension adjusting roller 33 may be directly driven by the air cylinder to move up by the second set distance in the longitudinal direction.
Example 4
The embodiment provides a preparation method of polyacrylonitrile-based carbon fiber, wherein a step of homogenizing polyacrylonitrile fiber is added after a step of filament withdrawing of polyacrylonitrile fiber and before a step of pre-oxidizing of polyacrylonitrile fiber in a preparation process of polyacrylonitrile-based carbon fiber. Wherein, the homogenization treatment device of the embodiment 1 or the embodiment 2 is adopted to carry out homogenization treatment on the polyacrylonitrile fibers; or the polyacrylonitrile fibers were homogenized by the homogenization method described in example 3.
Here, the preparation steps of the polyacrylonitrile-based carbon fiber proposed in this embodiment mainly include: preparing polyacrylonitrile fiber, homogenizing (spraying, tension balancing, drying and preheating), pre-oxidizing, carbonizing, surface treating, sizing and the like
Here, according to the preparation method of the polyacrylonitrile-based carbon fiber provided in this embodiment, after the step of drawing the polyacrylonitrile fiber and before the step of pre-oxidizing the polyacrylonitrile fiber in the preparation process of the polyacrylonitrile-based carbon fiber, the homogenization device and the method of the above embodiment are used to pre-oxidize the polyacrylonitrile fiber, so that the finally prepared polyacrylonitrile-based carbon fiber has a small coefficient of variation of the performance index.
The invention is further illustrated by specific comparative experiments below:
example 5
In example 5, a polyacrylonitrile-based carbon fiber is prepared, the polyacrylonitrile precursor specification in this example is T800H-12k, and the target value of tension adjustment is 400-:
as shown in figures 1 and 2, three steps of spraying, tension balancing and drying preheating are added between the step of fiber unwinding and the step of pre-oxidation of the polyacrylonitrile fiber. The spraying step adopts a spraying device which comprises a water tank 23, a spraying head 22 and a spraying main pipe 21. The tension balancing step uses a tension balancing device including a first guide roller 31, a second guide roller 32, and a tension adjusting roller 33. The drying preheating step employs a drying preheating device including a drying heat roller unit composed of 8 drying heat rollers 41. The water in the spraying device is sprayed to the surface of polyacrylonitrile fiber through a spraying header pipe 21 on a fixed spraying bracket and a spraying header 22, and then is gathered to a water tank 23. Two first guide rollers 31 and two second guide rollers 32 in the tension balancing device are fixed on the bracket and are respectively driven by a motor. Two rolling bearings are arranged at the two ends of the tension adjusting roller 33, and are simultaneously connected with a weight 37 in a water tank 38 through a transmission belt 34, and the longitudinal position of the tension adjusting guide roller 33 is adjusted through the self gravity of the tension adjusting roller 32 and the buoyancy change difference of the weight 37 in the water tank 38 so as to adjust the tension of the tows (see the content of example 2 for a specific adjusting method).
Meanwhile, the moisture formed by drying can be discharged to the outside through the waste hood 42. Wherein the spraying amount of the spraying device is 5L/min, the installed power of the tension balancing device (the motor transmission power of the first guide roller and the second guide roller) is 8kW, the installed power of the drying and preheating device is 96kW, the drying and preheating temperature is 80-150 ℃, and the total treatment time is 4 min.
Comparative example 1
Comparative example 1 a polyacrylonitrile-based carbon fiber was prepared, which is different from example 5 in the following preparation process: the three steps of spraying, tension balancing and drying and preheating are not required between the step of filament withdrawing and the step of pre-oxidation of the polyacrylonitrile fiber, and the polyacrylonitrile fiber after the step of filament withdrawing directly enters an oxidation furnace for reaction through a transmission roller.
The properties of the polyacrylonitrile fiber before pre-oxidation and the prepared polyacrylonitrile-based carbon fiber in example 5 and comparative example 1 were compared as follows:
(1) the performance of polyacrylonitrile fibers (precursor fibers of different stations) and polyacrylonitrile-based carbon fibers between different stations are compared, and the comparison is shown in table 1.
TABLE 1
Note: the statistical result is 5 batches, and each batch of 100-axis precursor and the corresponding carbon filament performance value are obtained.
(2) The performance of polyacrylonitrile fiber (precursor fiber of the same station long distance) and polyacrylonitrile-based carbon fiber of the same station long distance are compared, and see table 2.
TABLE 2
Note: the statistical result is 5 batches, and 10-axis precursor and corresponding carbon filament performance values of each batch are obtained.
It is apparent from the data in tables 1 and 2 that the water content index of the polyacrylonitrile fiber (precursor) and the performance index of the polyacrylonitrile-based carbon fiber are more uniform between different stations and in the long-range of the same station after the polyacrylonitrile fiber (precursor) is subjected to continuous homogenization treatment. Therefore, the invention meets the expected design target requirement and improves the economic benefit.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.
Claims (10)
1. A homogenization treatment device for homogenizing polyacrylonitrile fibers after a step of fiber withdrawal and before a step of pre-oxidation of the polyacrylonitrile fibers, characterized by comprising:
the spraying device is used for spraying water on the surface of the polyacrylonitrile fibers;
the drying and preheating device is used for drying and preheating the polyacrylonitrile fibers subjected to spraying treatment and keeping the polyacrylonitrile fibers at a set water content;
under the traction action of the transmission device, the polyacrylonitrile fiber is firstly sprayed by the spraying device and then dried and preheated by the drying and preheating device.
2. The homogenizing apparatus of claim 1, further comprising:
the tension balancing device is used for adjusting the tension of the polyacrylonitrile fiber and adjusting the tension value of the polyacrylonitrile fiber to a target tension value;
the polyacrylonitrile fiber sequentially passes through the spraying device, the tension balancing device and the drying and preheating device under the traction action of the transmission device; or
The polyacrylonitrile fiber passes through the tension balancing device, the spraying device and the drying and preheating device in sequence under the traction action of the transmission device.
3. Homogenizing treatment apparatus according to claim 1 or 2,
the spraying device comprises a spraying pipeline and a spraying head; the spraying head is connected with the spraying pipeline and is used for spraying water on the surface of the polyacrylonitrile fiber passing through the spraying device; preferably, the spraying device further comprises a water tank; wherein the water tank is positioned below the spray header; the polyacrylonitrile fiber passes through the spraying device between the spraying head and the water tank under the traction action of the transmission device; and/or
The drying preheating device comprises a plurality of drying hot rollers; the polyacrylonitrile fiber sequentially passes through a plurality of drying hot rollers in the drying and preheating device under the traction action of the transmission device; preferably, the homogenizing device further comprises a waste discharge cover for discharging water vapor generated during drying and preheating of the polyacrylonitrile fibers to the outside; preferably, the temperature of the drying thermo roll is adjusted in the range of 50 to 200 ℃.
4. Homogenizing treatment device according to claim 2, characterized in that the tension balancing device comprises: the tension adjusting device comprises a first guide roller, a tension adjusting roller, a second guide roller and an adjusting device; wherein,
the polyacrylonitrile fiber passes through a first guide roller, a tension adjusting roller and a second guide roller in sequence under the traction action of a transmission device; the polyacrylonitrile fiber which horizontally runs downwards longitudinally after being guided by the first guide roller; the polyacrylonitrile fiber which runs longitudinally downwards runs longitudinally upwards after being guided by the tension adjusting roller; the polyacrylonitrile fiber which runs longitudinally and upwards runs horizontally after being guided by the second guide roller;
the adjusting device is used for adjusting the position of the tension adjusting roller in the longitudinal direction so as to adjust the tension of the polyacrylonitrile fibers;
preferably, the tension adjusting range of the tension balancing device is 50-2000 cN.
5. Homogenizing treatment apparatus according to claim 4,
the adjusting device comprises a transmission belt, a water tank and a heavy object; wherein the weight is disposed in the water tank; one end of the transmission belt is connected with the tension adjusting roller, the transmission belt extends upwards, and the other end of the transmission belt is connected with the heavy object after being guided by the guide structure; the position of the weight when the stress is balanced is adjusted by adjusting the water storage capacity in the water tank, and the position of the tension adjusting roller in the longitudinal direction is further adjusted; or
The adjusting device comprises a driving mechanism, wherein the driving mechanism is connected with the tension adjusting roller and is used for adjusting the position of the tension adjusting roller in the longitudinal direction by driving the tension adjusting roller to move up or down; preferably, the drive mechanism comprises a pneumatic cylinder.
6. A homogenization treatment method is characterized in that the homogenization treatment is carried out on polyacrylonitrile fibers after the step of fiber withdrawing of the polyacrylonitrile fibers and before the step of pre-oxidation of the polyacrylonitrile fibers, wherein the homogenization treatment method comprises the following steps:
water spraying: carrying out water spraying treatment on polyacrylonitrile fibers so as to enable the surfaces of the polyacrylonitrile fibers to be attached with water;
drying and preheating: and drying and preheating the polyacrylonitrile fiber after the spraying treatment so as to dry the polyacrylonitrile fiber and keep the polyacrylonitrile fiber at a set water content.
7. The homogenization process of claim 6, wherein the step of homogenizing further comprises:
and (3) tension balance: performing tension adjustment on the polyacrylonitrile fiber to adjust the tension of the polyacrylonitrile fiber to a target value;
wherein the step of tension balancing is performed after the step of water spraying and before the step of drying and preheating; or the step of tension balancing is performed before the step of water spraying.
8. The method of homogenizing treatment according to claim 6 or 7, wherein the polyacrylonitrile fiber is homogenized by the homogenizing treatment apparatus according to any one of claims 1 to 5.
9. The method of claim 8, wherein when the homogenizing apparatus comprises a tension balancing apparatus, and the tension balancing apparatus comprises a first guide roller, a tension adjusting roller, a second guide roller, and an adjusting apparatus:
if the tension value of the polyacrylonitrile fiber is smaller than the target tension value, enabling the tension adjusting roller to longitudinally move downwards by a first set distance through the adjusting device when the polyacrylonitrile fiber passes through the tension balancing device;
and if the tension value of the polyacrylonitrile fiber is greater than the target tension value, enabling the tension adjusting roller to longitudinally rise for a second set distance through the adjusting device when the polyacrylonitrile fiber passes through the tension balancing device.
10. A preparation method of polyacrylonitrile-based carbon fiber is characterized by further comprising the following steps after the step of filament withdrawing of polyacrylonitrile fiber and before the step of pre-oxidation of the polyacrylonitrile fiber in the preparation process of the polyacrylonitrile-based carbon fiber: homogenizing polyacrylonitrile fibers; wherein,
homogenizing polyacrylonitrile fibers by using the homogenizing device of any one of claims 1 to 5; and/or
The polyacrylonitrile fiber is homogenized by the homogenizing method according to any one of claims 6 to 9.
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