CN111893668B - 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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- CN111893668B CN111893668B CN202010646779.XA CN202010646779A CN111893668B CN 111893668 B CN111893668 B CN 111893668B CN 202010646779 A CN202010646779 A CN 202010646779A CN 111893668 B CN111893668 B CN 111893668B
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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
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- 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
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- 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
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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
- 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, distillation
Abstract
The invention relates to a homogenizing treatment device and method and a preparation method of polyacrylonitrile-based carbon fibers, and relates to the technical field of carbon fibers. The technical scheme mainly adopted is as follows: a homogenizing treatment device is used for homogenizing the polyacrylonitrile fiber before the step of pre-oxidizing the polyacrylonitrile fiber, wherein the homogenizing treatment 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 sprayed polyacrylonitrile fibers and keeping the set water content of the polyacrylonitrile fibers. Under the traction action of the transmission device, the polyacrylonitrile fiber is sprayed by a spraying device and then is dried and preheated by a drying and preheating device. The invention mainly reduces the discrete coefficient of the water content 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 homogenizing 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%. It is widely used in the fields of aerospace, rail traffic, wind power generation, sports equipment and the like. The preparation process of the polyacrylonitrile-based carbon fiber comprises the following steps: the polyacrylonitrile fiber is prepared (the polyacrylonitrile fiber herein refers to a precursor of the polyacrylonitrile-based carbon fiber, and is also referred to as a "precursor" by those skilled in the art), and the polyacrylonitrile fiber is sequentially subjected to operations such as pre-oxidation, carbonization, surface treatment, sizing, and the like, to obtain the polyacrylonitrile-based carbon fiber.
At present, the main flow of the preoxidation process for the polyacrylonitrile fiber 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-removing creel. The prior art adds a preheating step between the step of the filament-removing of the polyacrylonitrile fiber and the step of the preoxidation of the polyacrylonitrile fiber so as to dehydrate and deoil the polyacrylonitrile fiber, thereby reducing the pollution of water and oiling agents to a preoxidation furnace.
However, the present inventors found that the existing polyacrylonitrile-based carbon fiber preparation process has at least the following problems: before the polyacrylonitrile fiber enters the oxidation furnace, the water content difference 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 further, the dispersion coefficient deviation of the mechanical properties of the polyacrylonitrile-based carbon fiber at different stations is large. Meanwhile, the prior art has less research on continuous homogenization treatment of polyacrylonitrile fibers.
Disclosure of Invention
In view of the above, the present invention provides a homogenizing device and method, and a method for preparing polyacrylonitrile-based carbon fiber, which mainly aims at: before the polyacrylonitrile fiber is subjected to pre-oxidation treatment, the water content discrete coefficient of the polyacrylonitrile fiber at different stations can be reduced.
The term "polyacrylonitrile fiber" in the present invention refers to a precursor of polyacrylonitrile-based carbon fiber, and is commonly referred to as "filament" by those skilled in the art.
In order to achieve the above purpose, the present invention mainly provides the following technical solutions:
in one aspect, an embodiment of the present invention provides a homogenizing apparatus for homogenizing a polyacrylonitrile fiber after a step of drawing back the polyacrylonitrile fiber and before a step of pre-oxidizing the polyacrylonitrile fiber, wherein the homogenizing apparatus includes:
the spraying device is used for spraying water on the surfaces of the polyacrylonitrile fibers;
the drying and preheating device is used for carrying out drying and preheating treatment on the polyacrylonitrile fibers after the spraying treatment and keeping the set water content of the polyacrylonitrile fibers;
and the polyacrylonitrile fiber is subjected to spray treatment through the spray device and then drying and preheating treatment through the drying and preheating device under the traction action of the transmission device.
Preferably, the homogenizing 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 be 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 (b)
And the polyacrylonitrile fiber sequentially passes through the tension balancing device, the spraying device and the drying and preheating device under the traction action of the transmission device.
Preferably, the spraying device comprises a spraying pipeline and a spraying head; the spray header is connected with the spray pipeline and is used for spraying water on the surface of the polyacrylonitrile fiber passing through the spray 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 and preheating device comprises a plurality of drying hot rolls; 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 treatment device further comprises a waste discharge cover for discharging water vapor generated during drying and preheating of the polyacrylonitrile fiber to the outside; preferably, the temperature of the drying hot roller is adjusted to 50-200 ℃.
Preferably, the tension balancing device includes: the device comprises a first guide roller, a tension adjusting roller, a second guide roller and an adjusting device; wherein, the liquid crystal display device comprises a liquid crystal display device,
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 horizontally running polyacrylonitrile fiber runs longitudinally downwards 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 upwards runs horizontally after being guided by the second guiding 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 fiber;
preferably, the tension balance device has a tension adjustment range of 50-2000cN.
Preferably, the adjusting device comprises a driving belt, a water tank and a weight; wherein the weight is disposed in the water tank; one end of the driving belt is connected with the tension adjusting roller, the driving belt extends upwards, and the other end of the driving belt is connected with the weight after being guided by the guide structure; the position of the weight when the weight is stressed and balanced is adjusted by adjusting the water storage capacity in the water tank, so that the position of the tension adjusting roller in the longitudinal direction is adjusted; or (b)
The adjusting device comprises a driving mechanism, wherein the driving mechanism is connected with the tension adjusting roller, and the position of the tension adjusting roller in the longitudinal direction is adjusted by driving the tension adjusting roller to move up or down; preferably, the driving mechanism includes a cylinder.
In another aspect, an embodiment of the present invention provides a homogenizing method, in which a polyacrylonitrile fiber is homogenized after a step of filament-removing the polyacrylonitrile fiber and before a step of pre-oxidizing the polyacrylonitrile fiber, wherein the homogenizing method includes the steps of:
spraying water: carrying out water spraying treatment on the 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 sprayed polyacrylonitrile fiber to dry the polyacrylonitrile fiber, and keeping the polyacrylonitrile fiber with a set water content.
Preferably, the step of homogenizing further comprises:
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 fiber is homogenized by the homogenizing apparatus according to any one of the above.
Preferably, when the homogenizing treatment device comprises a tension balancing device, and the tension balancing device comprises 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, longitudinally moving the tension adjusting roller downwards by a first set distance through the adjusting device when the polyacrylonitrile fiber passes through the tension balancing device;
if the tension value of the polyacrylonitrile fiber is larger than the target tension value, the tension adjusting roller is longitudinally lifted by a second set distance through the adjusting device when the polyacrylonitrile fiber passes through the tension balancing device.
In still another aspect, an embodiment of the present invention provides a method for preparing a polyacrylonitrile-based carbon fiber, which further includes, after a step of filament-removing the polyacrylonitrile fiber in a process of preparing the polyacrylonitrile-based carbon fiber, before a step of pre-oxidizing the polyacrylonitrile fiber: homogenizing the polyacrylonitrile fiber; wherein, the liquid crystal display device comprises a liquid crystal display device,
homogenizing the polyacrylonitrile fiber by using the homogenizing device of any one of the above; and/or
The polyacrylonitrile fiber is homogenized by the homogenization treatment method described in any one of the above.
Compared with the prior art, the homogenizing treatment device and method and the preparation method of the polyacrylonitrile-based carbon fiber have at least the following beneficial effects:
on one hand, according to the homogenizing treatment device and the homogenizing treatment method provided by the embodiment of the invention, a certain amount of water is uniformly attached to the surface of the polyacrylonitrile fiber through the spraying device, so that the hairline generated by the electrostatic action of the fiber can be reduced. And then drying the polyacrylonitrile fiber by a drying and preheating device, and controlling the polyacrylonitrile fiber to retain a certain water content at the same time so as to play a role in homogenizing the water content of the polyacrylonitrile fiber.
Further, according to the homogenizing treatment device and the homogenizing treatment method provided by the embodiment of the invention, the tension of the polyacrylonitrile fiber is regulated through the tension balancing device, so that the tension of the polyacrylonitrile fiber at different stations is kept consistent, and finally, under the action of the drying hot roller, the water-containing homogenizing 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 finally, the problem that the dispersion coefficient of the performance index of the polyacrylonitrile-based carbon fiber is larger is solved.
On the other hand, according to the polyacrylonitrile-based carbon fiber provided by the embodiment of the invention, the step of homogenizing the polyacrylonitrile fiber is added after the step of filament-removing the polyacrylonitrile fiber in the preparation process of the polyacrylonitrile-based carbon fiber and before the step of pre-oxidizing the polyacrylonitrile fiber, so that the 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 present invention, and is intended to provide a better understanding of the present invention, as it is embodied in the following description, with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
Fig. 1 is a schematic structural view of a homogenizing treatment apparatus according to an embodiment of the present invention;
fig. 2 is a flow chart of a homogenization treatment method according to an embodiment of the present invention.
Detailed Description
In order to further describe the technical means and effects adopted for achieving the preset aim of the invention, the following detailed description refers to the specific implementation, structure, characteristics and effects according to the application of the invention with reference to the accompanying drawings and preferred embodiments. In the following description, different "an embodiment" or "an embodiment" do not necessarily refer to the same embodiment. Furthermore, the particular features, structures, or characteristics of one or more embodiments may be combined in any suitable manner.
Example 1
In one aspect, the present embodiment provides a homogenizing apparatus for homogenizing a polyacrylonitrile fiber after a step of filament-removing the polyacrylonitrile fiber and before a step of pre-oxidizing the polyacrylonitrile fiber. As shown in fig. 1, the homogenizing 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 sprayed polyacrylonitrile fibers 1 and keeping the polyacrylonitrile fibers 1 at a set water content. Under the traction action of the transmission device, the polyacrylonitrile fiber 1 is sprayed by a spraying device and then is dried and preheated by a drying and preheating device.
Preferably, the spraying device comprises a spraying pipeline 21 and a spraying head 22; wherein the spray header 22 is connected with the spray pipeline 21 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 and preheating means includes a plurality of drying heat rolls 41; wherein, the polyacrylonitrile fiber 1 passes through a plurality of drying hot rolls 41 in the drying and preheating device in turn under the traction action of the transmission device. Preferably, the number of the drying heat rollers 41 is 8.
Preferably, the homogenizing treatment apparatus further comprises a waste cover 42 for discharging moisture generated during drying and preheating of the polyacrylonitrile fiber to the outside. Wherein the temperature of the drying hot roller is regulated to be 50-200 ℃.
In this embodiment, the homogenizing treatment device provided by the present invention makes the surface of the polyacrylonitrile fiber uniformly adhere to a certain amount of water through the spraying device, so that the filigree generated by the electrostatic action of the fiber can be reduced. And then, after the temperature of the hot roller is optimally set according to a certain temperature gradient through a drying and preheating device, the polyacrylonitrile fiber is dried, so that certain water content of the polyacrylonitrile fiber at different stations is ensured to be reserved, the control range of the water content is generally 0.7-0.9%, and the water content homogenization effect is realized on the polyacrylonitrile fiber. The above-mentioned temperature optimization setting of the heat roller according to a certain temperature gradient means that in the drying and preheating device, the temperature of the latter heat roller is 10-20 ℃ higher than the temperature of the former drying heat roller. Wherein the temperature of the initial heat roller is generally 50-70 ℃ and the temperature of the final heat roller is 170-200 ℃. After the drying and preheating step, manual sampling and inspection are performed before entering the oxidation furnace.
Here, the polyacrylonitrile fiber is controlled to keep a certain water content, and has the following positive effects: in the early stage of pre-oxidation, the moisture in the polyacrylonitrile fiber is combined with oxygen-containing functional groups generated by the reaction of the polyacrylonitrile fiber, so that the mutual entanglement of molecular chains in the fiber structure is enhanced, the reaction capacity of partial macromolecular chain segments is frozen, the cyclization reaction rate is eased 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, simultaneously, micro holes are formed on the surface of the fiber by water, the entry of oxygen and the escape of wastes generated by the reaction are facilitated, 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 = (sample tow-oven dried tow)/oven dried tow x 100%.
If the polyacrylonitrile fiber contains excessive moisture, the reaction rate of the degree of cyclization of the polyacrylonitrile fiber is too low. The cyclization degree is the premise that oxidation reaction occurs, the oxidation reaction occurs to a lower degree, the insufficient pre-oxidation degree of the fiber is finally caused, the sheath-core structure of the pre-oxidized fiber is overlarge, the homogenization degree of the fiber is reduced, and the performance is reduced.
Therefore, the consistency of the pre-oxidation degree of the polyacrylonitrile fibers at different stations can be improved by controlling the water content of the polyacrylonitrile fibers to be kept at a set amount, and the homogenization of the polyacrylonitrile-based carbon fibers can be further improved.
Example 2
Preferably, the present embodiment provides a homogenizing apparatus, as shown in fig. 1, where the homogenizing apparatus further includes a tension balancing device for adjusting the tension of the polyacrylonitrile fiber to adjust 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 tension balancing device in the present embodiment includes: the first guide roller 31, the tension adjusting roller 33, the second guide roller 32 and the 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 the first guide roller 31, the tension adjusting roller 33 and the second guide roller 32 in sequence under the traction action of the transmission device. The horizontally running polyacrylonitrile fiber runs longitudinally downwards 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 which runs longitudinally upward runs horizontally after being guided by the second guide roller 32. Wherein the adjusting means 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 up or down in the longitudinal direction by the adjusting means) to adjust the tension of the polyacrylonitrile fiber. Preferably, the tension balance device has a tension adjustment range of 50-2000cN.
Further preferably, the adjusting device in the present embodiment is configured as follows:
the adjusting means comprises a drive belt 34, a water tank 38 and a weight 37. The weight 37 is placed in the water tank 38. One end of the driving belt 34 is connected to the tension adjusting roller 33, and after the driving belt extends upward (i.e., the end of the driving belt connected to the tension adjusting roller 33 is the lower end), the other end of the driving 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 being stressed and balanced is adjusted by adjusting the water storage amount in the water tank 38, and the position of the tension adjusting roller 33 in the longitudinal direction is further adjusted.
For example: (1) The target tension value for the running tow is 2000cN, while the current tension value for the tow at the tension balancing device is 1500cN. Here, by injecting water into the water tank 38, the buoyancy generated by the weight 37 gradually increases as the water level increases, at this time, the tension of the tension adjusting roller to which the weight is subjected plus the buoyancy greater than the gravity of the weight itself, the weight 38 gradually floats up under the action of the belt 34, the tension adjusting roller 33 sinks, the draft tension carried by the tow increases, and when the tension adjusting roller 33 and the weight 37 reestablish balance, the displacement of the tension adjusting roller 37 falling is h, and the displacement of the weight 37 rising is h, thereby realizing the adjustment of the tension of the tow. (2) When the running tow tension target value is 2000cN, the current tow tension value at the tension balancing device is 2500cN. By draining the water tank 38, the buoyancy generated by the weight 37 gradually decreases as the water tank level decreases, at this time, the tension of the tension adjusting roller borne by the weight plus the buoyancy borne by the weight is smaller than the gravity of the weight itself, the weight 37 gradually sinks under the action of the transmission belt, the tension adjusting roller 33 rises, the drafting tension borne by the tow decreases, when the tension adjusting roller 33 and the weight 37 reestablish balance, the rising displacement of the tension adjusting roller 33 becomes h, the falling displacement of the weight 37 becomes h, and the adjustment of the tow tension is realized. In the normal state, the tension of the filament bundle increases by 100cN every 0.5cm of the tension adjusting roller 33 is lowered.
In addition, the adjusting device may be designed as follows, in addition to the above-described structure: the adjusting device includes a driving mechanism, wherein the driving mechanism is connected with the tension adjusting roller 33, and adjusts the position of the tension adjusting roller 33 in the longitudinal direction by driving the tension adjusting roller 33 to move up or down. The driving mechanism includes a cylinder, and the tension adjusting roller 33 is driven to rise or fall by the cylinder.
In summary, the homogenizing treatment device provided in this embodiment adjusts the tension of the polyacrylonitrile fiber through the tension balancing device, so that the tension of the polyacrylonitrile fiber at different stations is kept consistent, and finally, under the action of the drying hot roller, the water-containing homogenizing effect is performed on the precursor, so that the performance of the polyacrylonitrile fiber before entering the oxidation furnace is kept consistent, and finally, the problem that the performance index discrete coefficient of the carbon fiber is larger is solved.
Preferably, the homogenizing treatment device in the above embodiment further comprises a homogenizing treatment chamber, and the spraying device, the tension balancing device and the drying preheating device are all arranged in the homogenizing treatment 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 to be sequentially sprayed, balanced in tension, dried and preheated (or balanced in tension, sprayed and dried and preheated), and then are pulled out from the tow outlet.
Example 3
On the other hand, the present embodiment provides a homogenizing method for homogenizing a polyacrylonitrile fiber after the step of filament-removing the polyacrylonitrile fiber and before the step of pre-oxidizing the polyacrylonitrile fiber, as shown in fig. 2. The homogenizing treatment method comprises the following steps:
spraying water: and carrying out water spraying treatment on the 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 sprayed polyacrylonitrile fiber to dry the polyacrylonitrile fiber, and keeping the polyacrylonitrile fiber with a set water content.
Preferably, the step of homogenizing further comprises:
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 homogenizing treatment method provided by the embodiment, a layer of water is uniformly adhered to the surface of the precursor through a spraying step, the tension of the precursor at different stations is kept consistent through the adjustment of the tension balancing device, and finally, the precursor is subjected to water-containing homogenizing under the action of the drying hot roller, so that the uniformity of the performance of the precursor before entering the oxidation furnace is kept, and finally, the problem of larger dispersion coefficient of the performance index of the carbon fiber is solved.
Preferably, the polyacrylonitrile fiber is homogenized by the homogenizing apparatus described in example 1 and example 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, the tension adjusting roller 33 is moved longitudinally downward by a first set distance by the adjusting device when the polyacrylonitrile fiber 1 passes through the tension balancing device.
As shown in fig. 1, water may be supplied to the water tank 38 to raise the weight 37 a first set distance, and the tension adjusting roller 33 is moved longitudinally downward by the first set distance by the belt 34.
Of course, the tension adjusting roller 33 may be directly driven by an air cylinder to longitudinally move downward by a first set distance.
(2) If the tension value of the polyacrylonitrile fiber is larger than the target tension value, the tension adjusting roller is longitudinally lifted by 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 by a second set distance, and the tension adjusting roller 33 may be raised longitudinally by the second set distance by the belt 34.
Of course, the tension adjusting roller 33 may be directly driven by the cylinder to longitudinally move upward by a second set distance.
Example 4
The embodiment provides a preparation method of polyacrylonitrile-based carbon fiber, wherein a step of homogenizing the polyacrylonitrile fiber is added after a step of filament-removing the polyacrylonitrile fiber in the preparation process of the polyacrylonitrile-based carbon fiber and before a step of pre-oxidizing the polyacrylonitrile fiber. Wherein the homogenization treatment device described in example 1 or example 2 was used to homogenize the polyacrylonitrile fiber; or the homogenization treatment method described in example 3.
The preparation steps of the polyacrylonitrile-based carbon fiber provided 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, since the preparation method of the polyacrylonitrile-based carbon fiber provided in this embodiment employs the homogenization treatment device and method of the above embodiment to pre-oxidize the polyacrylonitrile fiber after the step of filament removal of the polyacrylonitrile fiber and before the step of pre-oxidizing the polyacrylonitrile fiber in the preparation process of the polyacrylonitrile-based carbon fiber, the performance index dispersion coefficient of the finally prepared polyacrylonitrile-based carbon fiber is small.
The invention is further illustrated by the following specific comparative experiments:
example 5
Example 5 a polyacrylonitrile-based carbon fiber was prepared, the polyacrylonitrile precursor in this example had a specification of T800H-12k, and the target value of tension adjustment was 400-600cN, and compared with the conventional process for preparing a polyacrylonitrile-based carbon fiber, example 5 adds a step of homogenizing a polyacrylonitrile fiber after the step of annealing a polyacrylonitrile fiber and before the step of pre-oxidizing a polyacrylonitrile fiber, specifically as follows:
as shown in fig. 1 and 2, three steps of spraying, tension balancing and drying and preheating are added between the step of filament drawing and the step of pre-oxidizing the polyacrylonitrile fibers. The spraying step adopts a spraying device which comprises a water tank 23, a spray header 22 and a spray header 21. The tension balancing step adopts a tension balancing device which comprises a first guide roller 31, a second guide roller 32 and a tension adjusting roller 33. The drying and preheating step adopts a drying and preheating device which comprises a drying and hot roller unit consisting of 8 drying and hot rollers 41. The water in the spray device is sprayed to the surface of the polyacrylonitrile fiber through a spray header 22 by a spray header 21 on the fixed spray bracket and is gathered to a water tank 23. In the tension balancing device, two first guide rollers 31 and two second guide rollers 32 are fixed on a bracket and are driven by motors respectively. Two rolling bearings are arranged at the two ends of the tension adjusting roller 33 and are connected with a weight 37 in a water tank 38 through a driving 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 value of the weight 37 in the water tank 38 so as to adjust the tension of the tows (the specific adjusting method is shown in the content of the embodiment 2).
Meanwhile, the moisture formed by the drying may be discharged to the outside through the exhaust hood 42. 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 4min.
Comparative example 1
Comparative example 1 a polyacrylonitrile-based carbon fiber was prepared, and the preparation process thereof was different from that of example 5 in that: the three steps of spraying, tension balancing and drying and preheating are not carried out between the step of filament drawing and the step of preoxidation of the polyacrylonitrile fiber, and the polyacrylonitrile fiber after the step of filament drawing directly enters an oxidation furnace through a transmission roller for reaction.
The properties of the polyacrylonitrile fiber before preoxidation and the prepared polyacrylonitrile-based carbon fiber in example 5 and comparative example 1 were compared as follows:
(1) The properties of the polyacrylonitrile fiber (precursor of different stations) and the polyacrylonitrile-based carbon fiber between different stations are compared, and are shown in table 1.
TABLE 1
Note that: the statistical result is 5 batches, each batch of 100-axis precursor and the corresponding carbon filament performance value.
(2) The properties of the polyacrylonitrile fiber (the precursor of the same station) and the polyacrylonitrile-based carbon fiber are compared, and are shown in table 2.
TABLE 2
Note that: the statistical result is 5 batches, 10 axis precursors of each batch and the corresponding carbon filament performance value.
As is apparent from the data in tables 1 and 2, 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 on the same station long distance after the continuous homogenization treatment of the polyacrylonitrile fiber (precursor). Therefore, the invention meets the expected design target requirement and improves the economic benefit.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention in any way, but any simple modification, equivalent variation and modification made to the above embodiments according to the technical substance of the present invention still fall within the scope of the technical solution of the present invention.
Claims (7)
1. A homogenizing apparatus for homogenizing a polyacrylonitrile fiber after a step of filament-removing the polyacrylonitrile fiber and before a step of pre-oxidizing the polyacrylonitrile fiber, the homogenizing apparatus comprising:
the spraying device is used for spraying water on the surfaces of the polyacrylonitrile fibers;
the drying and preheating device is used for carrying out drying and preheating treatment on the polyacrylonitrile fibers after the spraying treatment and keeping the set water content of the polyacrylonitrile fibers;
under the traction action of a transmission device, the polyacrylonitrile fiber is sprayed by the spraying device and then dried and preheated by the drying and preheating device;
the drying and preheating device comprises a plurality of drying hot rolls; 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; wherein the temperature regulation range of the drying hot roller is 50-200 ℃, and in the drying preheating device, the temperature of the latter hot roller is 10-20 ℃ higher than the temperature of the former drying hot roller; wherein the temperature of the initial hot roller is 50-70 ℃, and the temperature of the final hot roller is 170-200 ℃;
wherein the homogenizing treatment device 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 be 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;
wherein, the tension balancing device includes: the device comprises a first guide roller, a tension adjusting roller, a second guide roller and an adjusting device; the polyacrylonitrile fiber passes through the first guide roller, the tension adjusting roller and the second guide roller in sequence under the traction action of the transmission device; the horizontally running polyacrylonitrile fiber runs longitudinally downwards 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 upwards runs horizontally after being guided by the second guiding 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 fiber;
wherein the adjusting device comprises a driving belt, a water tank and a weight; wherein the weight is disposed in the water tank; one end of the driving belt is connected with the tension adjusting roller, the driving belt extends upwards, and the other end of the driving belt is connected with the weight after being guided by the guide structure; the position of the weight is adjusted when the weight is stressed and balanced by adjusting the water storage capacity in the water tank, so that the position of the tension adjusting roller in the longitudinal direction is adjusted.
2. A homogenizing treatment apparatus as claimed in claim 1, wherein,
the spraying device comprises a spraying pipeline and a spraying head; the spray header is connected with the spray pipeline and used for spraying water on the surface of the polyacrylonitrile fiber passing through the spray device.
3. A homogenizing treatment apparatus as claimed in claim 2, wherein,
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.
4. A homogenizing treatment apparatus as claimed in claim 1, wherein,
the homogenizing treatment device further comprises a waste discharge cover for discharging water vapor generated by drying and preheating the polyacrylonitrile fibers to the outside.
5. The homogenizing treatment apparatus of claim 1 wherein the tension balancing apparatus has a tension adjustment range of 50-2000cN.
6. A homogenizing method for homogenizing a polyacrylonitrile fiber after a step of filament-removing the polyacrylonitrile fiber and before a step of pre-oxidizing the polyacrylonitrile fiber, wherein the homogenizing method comprises the steps of:
spraying water: carrying out water spraying treatment on the polyacrylonitrile fibers so as to enable the surfaces of the polyacrylonitrile fibers to be attached with water;
drying and preheating: drying and preheating the sprayed polyacrylonitrile fiber to dry the polyacrylonitrile fiber, and keeping the polyacrylonitrile fiber with a set water content; wherein the polyacrylonitrile fiber is subjected to a homogenization treatment by the homogenization treatment apparatus as described in any one of claims 1 to 5;
wherein the step of homogenizing further comprises:
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;
if the tension value of the polyacrylonitrile fiber is smaller than the target tension value, longitudinally moving the tension adjusting roller downwards by a first set distance through the adjusting device when the polyacrylonitrile fiber passes through the tension balancing device; if the tension value of the polyacrylonitrile fiber is larger than the target tension value, the tension adjusting roller is longitudinally lifted by a second set distance through the adjusting device when the polyacrylonitrile fiber passes through the tension balancing device.
7. The preparation method of the polyacrylonitrile-based carbon fiber is characterized by further comprising the following steps of the step of filament removal of the polyacrylonitrile fiber and the step of preoxidation of the polyacrylonitrile fiber in the preparation process of the polyacrylonitrile-based carbon fiber: homogenizing the polyacrylonitrile fiber; wherein, the liquid crystal display device comprises a liquid crystal display device,
homogenizing polyacrylonitrile fiber with the homogenizing apparatus of any one of claims 1 to 5; and/or
A method of homogenizing a polyacrylonitrile fiber according to claim 6.
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