CN114262956B - Carbonization yarn splicing method for large-tow carbon fiber precursor - Google Patents

Carbonization yarn splicing method for large-tow carbon fiber precursor Download PDF

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CN114262956B
CN114262956B CN202111640924.4A CN202111640924A CN114262956B CN 114262956 B CN114262956 B CN 114262956B CN 202111640924 A CN202111640924 A CN 202111640924A CN 114262956 B CN114262956 B CN 114262956B
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precursor
fiber
precursor fiber
pan
oxidation
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CN114262956A (en
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闫学军
斛小晋
周东福
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Jilin Guoxin Carbon Fiber Co.,Ltd.
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Jilin Baojing Carbon Material Co ltd
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Abstract

The invention discloses a large-tow carbon fiber precursor carbonization yarn splicing method, which comprises the following steps: s1: a reticular cylindrical structure formed by interweaving acrylonitrile/Itaconic Acid (IA) binary copolymerization filaments is used as a PAN precursor filament cylinder, and a reserved spinneret and the PAN precursor filament cylinder are oxidized: untwisting the tail end of the precursor fiber and the head of the other precursor fiber to finish a 300-400mm spinneret, sleeving a PAN precursor fiber cylinder on the tail end of the precursor fiber, laying on an oxidation frame, and naturally tensioning and fixing the precursor fiber; s2: an air splicer is used for connecting the middle sections of the oxidation sections of the precursor fiber bundle head and the bundle tail. According to the invention, a method of pre-oxidizing the head and the tail of the precursor fiber tube is adopted, the PAN precursor fiber tube is used for buckling and connecting the first precursor fiber tube with the reserved spinneret of the second precursor fiber tube, and the first precursor fiber tube and the second precursor fiber tube are connected into a fiber bundle, so that the continuous carbonization of the large fiber bundle carbon fiber is realized.

Description

Carbonization yarn splicing method for large-tow carbon fiber precursor
Technical Field
The invention relates to the technical field of carbon fiber production, in particular to a carbonization yarn splicing method for large-tow carbon fiber precursors.
Background
The carbon fiber has the large and small tows, and in the application process of the carbon fiber, the small tows are mainly applied to the aerospace field, and in the industrial field, in order to realize the cost reduction, more large tows are needed, and at present, the large tows are already applied to some important civil fields. Such as infrastructure, sports equipment, fan blades, and automotive manufacturing, the research of the application of large tow carbon fibers is of great interest.
In the production of carbon fibers, the packaging of the precursor yarn, whether the yarn spindle or the box packaging, has a certain weight and length, and after the use, the new precursor yarn spindle and the box packaging need to be replaced, and the process is usually discontinuous, namely the production line is stopped, all precursor yarn packages (yarn spindles or box packaging) are replaced at one time, and the replaced precursor yarn is subjected to the oxidation and carbonization processes. Or in the continuous case, the oxidation furnace in the pre-oxidation process is cooled to enable the joint tows (the tail parts of the tows) to smoothly pass through the pre-oxidation, but the tows are reconnected in the carbonization part (the two tows packaged by the precursor are knotted or connected together in other modes), so that the production line is required to be stopped, and continuous and stable production is difficult in any mode.
In the above process, when a large tow is used, the continuous production mode is difficult, and when the large tow enters the oxidation process, any overturning and twisting or splicing of the precursor filaments (the splicing, i.e. knotting and connecting the two tows together) can lead to the heat release of the tows to be concentrated, smoke and fire to cause the tows to be broken. The length of the large tows is far smaller than that of the small tows when the same weight of the raw tows is packaged, and the length of the production line is very long. Therefore, continuous production is necessary for large-tow carbon fiber production.
In view of the above, the present invention provides a method for carbonizing and splicing large-strand carbon fiber precursor, which solves the problem that large-strand carbon fiber (above 48K) cannot be continuously produced at present, and aims to solve the problem and improve the practical value by the technology, and the precursor needs to be packaged (whether in a spindle, a box or a package) end to end, so that the precursor and the precursor are spliced and the precursor are connected together, and the continuous production is difficult to realize without breaking the oxidization and carbonization processes from the experience in the world.
Disclosure of Invention
The present invention aims to solve one of the technical problems existing in the prior art or related technologies.
The technical scheme adopted by the invention is as follows: a carbonization yarn splicing method for large-tow carbon fiber precursors comprises the following steps:
s1: reservation spinneret and PAN precursor cartridge oxidation: untwisting the tail end of the precursor fiber and the head of the other precursor fiber to finish a 300-400mm spinneret, sleeving a PAN precursor fiber cylinder on the tail end of the precursor fiber, laying on an oxidation frame, and naturally tensioning and fixing the precursor fiber;
s2: connecting the middle sections of the oxidation sections of the precursor fiber bundle head and the bundle tail by using an air splicer, straightening the expansion joint, moving the PAN precursor fiber cylinder to the connecting position for wrapping, and splicing the two ends of the PAN precursor fiber cylinder with the surfaces of the bundle head and the bundle tail by using the air splicer again;
s3: the completed spinneret part and the PAN precursor cartridge were connected, and the oxidation rack was put into an oven for oxidation and cooling.
The present invention may be further configured in a preferred example to: the reserved wire head and the PAN precursor wire barrel oxidation continuous pre-oxidation furnace are divided into 10 temperature areas, the temperature of each temperature area is set to be a constant value, the temperature of the furnace area is increased in a step manner, and the operating temperature of the fiber from the low-temperature furnace area to the high-temperature furnace area is changed within the range of 120-300 ℃.
By adopting the technical scheme, the pre-oxidation time is 60-120 min, and the density after pre-oxidation is 1.30-1.35 g/cm 3 Pre-oxidation of the AN precursor is carried out in air, and the reserved spinneret and the PAN precursor cylinder are oxidized, so that subsequent carbonization and bonding are facilitated.
The present invention may be further configured in a preferred example to: the PAN precursor wire cylinder is of a net-shaped cylindrical structure formed by interweaving acrylonitrile/itaconic acid (I A) binary copolymerization precursor wires, and the length of the PAN precursor wire cylinder is 350-400mm.
Through adopting above-mentioned technical scheme, remove PAN precursor silk section of thick bamboo to junction parcel, utilize the precursor to wrap up and carbonization joint to big silk bundle carbon fiber air twist joint to improve joint strength.
The present invention may be further configured in a preferred example to: in S2, after the PAN precursor fiber cylinder moves to the connecting position, twisting tows at two ends of the PAN precursor fiber cylinder, and limiting the PAN precursor fiber cylinder to an air splicing position through twisting.
The present invention may be further configured in a preferred example to: in step S3, nitrogen gas having a nitrogen content of 99.99% is cooled and filled.
By adopting the technical scheme, the PAN precursor silk cylinder and the end silk bundles jointly carry out cyclization reaction, the dehydrogenation reaction enables the raised surface textures to be overlapped and overlapped more fully, and on the other hand, the change of the molecular chain structure in pre-oxidation and carbonization causes the surface from the precursor silk to the carbon fiber to become gradually smooth due to the reduction of the macromolecular chain spacing, and the number of overlapping grooves on the surfaces of the PAN precursor silk cylinder and the end silk bundles is gradually reduced, so that the connection is gradually tight.
The beneficial effects obtained by the invention are as follows:
1. according to the invention, the continuous carbonization of the large-tow carbon fibers is realized by using the method of preoxidation of the head and the tail of the precursor fiber tube, using the PAN precursor fiber tube to carry out buckling connection on the tail fiber of the first precursor fiber tube and the reserved wire head of the second precursor fiber tube, and connecting the tail fiber of the first precursor fiber tube and the reserved wire head of the second precursor fiber tube into a single tow.
2. According to the invention, a PAN precursor fiber cylinder structure is adopted, and precursor is utilized to wrap and carbonize the large-tow carbon fiber air twisting points, so that the strength of the connecting points is improved.
Drawings
FIG. 1 is a schematic diagram of an infrared absorption spectrum of a PAN wire cylinder after 25-150deg.C treatment in accordance with one embodiment of the present invention;
fig. 2 is a schematic view of the structure of a PAN precursor cartridge according to an embodiment of the present invention.
Detailed Description
The objects, technical solutions and advantages of the present invention will become more apparent by the following detailed description of the present invention with reference to the accompanying drawings. It should be noted that, without conflict, the embodiments of the present invention and features in the embodiments may be combined with each other.
It is to be understood that this description is merely exemplary in nature and is not intended to limit the scope of the present invention.
A method for carbonizing a large-tow carbon fiber precursor provided in accordance with some embodiments of the present invention is described below with reference to the accompanying drawings.
The invention provides a large-tow carbon fiber precursor carbonization yarn splicing method, which comprises the following steps:
s1: reservation spinneret and PAN precursor cartridge oxidation: untwisting the tail end of the precursor fiber and the head of the other precursor fiber to finish a 300-400mm spinneret, sleeving a PAN precursor fiber cylinder on the tail end of the precursor fiber, laying on an oxidation frame, and naturally tensioning and fixing the precursor fiber;
s2: connecting the middle sections of the oxidation sections of the precursor fiber bundle head and the bundle tail by using an air splicer, straightening the expansion joint, moving the PAN precursor fiber cylinder to the connecting position for wrapping, and splicing the two ends of the PAN precursor fiber cylinder with the surfaces of the bundle head and the bundle tail by using the air splicer again;
s3: the completed spinneret part and the PAN precursor cartridge were connected, and the oxidation rack was put into an oven for oxidation and cooling.
In this embodiment, the reservation filament head and PAN filament tube oxidation continuous pre-oxidation furnace are divided into 10 temperature zones, the temperature of each temperature zone is set to be a constant value, the temperature of the furnace zone is increased in steps, and the operating temperature of the fiber from the low temperature furnace zone to the high temperature furnace zone is changed within the range of 120-300 ℃.
The copolymerization PAN silk tube starts to perform cyclization reaction at 120 ℃ to generate conjugated-C=N-structure, and simultaneously, slowly performs dehydrogenation reaction to generate conjugated-C=C-structure; copolymerization of PAN fibers at 190 ℃ results in severe cyclodehydration reaction to produce unsaturated aromatic ring structures.
Specifically, the pre-oxidation time is 60-120 min, and the density after pre-oxidation is 1.30-1.35 g/cm 3 Pre-oxidation of the AN precursor is carried out in air, and the reserved spinneret and the PAN precursor cylinder are oxidized, so that subsequent carbonization and bonding are facilitated.
In this example, the PAN precursor wire cylinder is a net-shaped cylinder structure formed by interweaving acrylonitrile/Itaconic Acid (IA) binary copolymerization precursor wires, and as shown in figure 2, the length of the PAN precursor wire cylinder is 350-400mm.
In this embodiment, in S2, the PAN precursor yarn packages are twisted after moving to the connection, and the PAN precursor yarn packages are limited to the air splice by twisting.
Specifically, the PAN precursor fiber cylinder is moved to the connecting position for wrapping, and the precursor fiber is utilized to wrap and carbonize the large-tow carbon fiber air twisting point, so that the strength of the wire connecting point is improved.
In this example, nitrogen gas having a nitrogen content of 99.99% is filled in the cooling in step S3.
Specifically, the PAN precursor fiber tube and the end fiber bundle jointly perform cyclization reaction, the dehydrogenation reaction enables the raised surface textures to be overlapped and overlapped more fully, on the other hand, the change of the molecular chain structure in pre-oxidation and carbonization causes the surface from the precursor fiber to the carbon fiber to become gradually smooth, and the number of overlapping grooves on the surfaces of the PAN precursor fiber tube and the end fiber bundle is gradually reduced, so that connection is gradually tight.
The air connector can refer to the fourth-stage air splicing mechanism of the eighteenth volume of the textile journal and the development direction of the air splicer, and is published by China university of textile, li Zhifeng and Chen Ruiqi, and can also use an air coupler produced by TEXKI MP in the United kingdom or an air coupler of Italy MESDAN.
In the present invention, the term "plurality" means two or more, unless explicitly defined otherwise. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items. The terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; "coupled" may be directly coupled or indirectly coupled through intermediaries. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
It will be understood that when an element is referred to as being "mounted," "secured" or "disposed" on another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "upper," "lower," "left," "right," and the like are used herein for illustrative purposes only and are not meant to be the only embodiment.
In the description of the present specification, the terms "one embodiment," "some embodiments," "particular embodiments," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.

Claims (6)

1. The carbonization yarn splicing method for the large-tow carbon fiber precursor is characterized by comprising the following steps of:
s1: a reticular cylindrical structure formed by interweaving acrylonitrile/Itaconic Acid (IA) binary copolymerization filaments is used as a PAN precursor filament cylinder, and a reserved spinneret and the PAN precursor filament cylinder are oxidized: untwisting the tail end of the precursor fiber and the head of the other precursor fiber to finish a 300-400mm spinneret, sleeving a PAN precursor fiber cylinder on the tail end of the precursor fiber, laying on an oxidation frame, and naturally tensioning and fixing the precursor fiber;
s2: connecting the middle sections of the oxidation sections of the precursor fiber bundle head and the bundle tail by using an air splicer, straightening the expansion joint, moving the PAN precursor fiber cylinder to the connecting position for wrapping, and splicing the two ends of the PAN precursor fiber cylinder with the surfaces of the bundle head and the bundle tail by using the air splicer again;
s3: the completed spinneret part and the PAN precursor cartridge were connected, and the oxidation rack was put into an oven for oxidation and cooling.
2. The method for carbonizing and splicing large-tow carbon fiber precursors according to claim 1, wherein the reserved spinneret and the PAN precursor tube oxidation continuous pre-oxidation furnace are divided into 10 temperature areas, the temperature of each temperature area is set to be a constant value, the temperature of the furnace area is increased in a step manner, and the operating temperature of the fiber from the low-temperature furnace area to the high-temperature furnace area is changed within the range of 120-300 ℃.
3. The method for carbonizing and splicing large-strand carbon fiber precursor according to claim 2, wherein the pre-oxidation time is60-120 min, and the density after pre-oxidation is 1.30-1.35 g/cm 3
4. A large tow carbon fiber precursor carbonization process according to claim 1 wherein said PAN precursor canister length is 350-400mm.
5. The method for carbonizing and splicing large-tow carbon fiber precursors according to claim 1, wherein in S2, the tows at both ends of the PAN precursor fiber canister are twisted after the PAN precursor fiber canister is moved to the junction, and the PAN precursor fiber canister is limited to the air splice by twisting.
6. The method for carbonizing large-strand carbon fiber precursor according to claim 1, wherein nitrogen gas having a nitrogen content of 99.99% is filled in the cooling step S3.
CN202111640924.4A 2021-12-29 2021-12-29 Carbonization yarn splicing method for large-tow carbon fiber precursor Active CN114262956B (en)

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CN1639804A (en) * 2002-02-25 2005-07-13 皇家飞利浦电子股份有限公司 Conductive fiber
CN101049991A (en) * 2007-05-09 2007-10-10 山东大学 Method for preparing bush of Nano TiO2 fiber
JP2010133074A (en) * 2008-11-10 2010-06-17 Toray Ind Inc Fiber pieced part and method for producing carbon fiber having the pieced part
JP2010255168A (en) * 2009-03-31 2010-11-11 Toray Ind Inc Process for producing carbon fiber
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CN208201201U (en) * 2018-05-22 2018-12-07 浙江精功碳纤维有限公司 A kind of carbon fiber continuous production wears the device that furnace connects silk
CN110387602A (en) * 2019-08-16 2019-10-29 广州赛奥碳纤维技术有限公司 A kind of the pre-oxidation equipment and silk head connection method of polyacrylonitrile fibril silk head
CN212560549U (en) * 2020-03-27 2021-02-19 华祥(中国)高纤有限公司 Polyester yarn end-to-end connecting device

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KR101164753B1 (en) * 2008-04-18 2012-07-12 미츠비시 레이온 가부시키가이샤 Production system and production method of carbon fiber thread
WO2010053170A1 (en) * 2008-11-10 2010-05-14 東レ株式会社 Fiber bundle with pieced part, process for producing same, and process for producing carbon fiber
US9884740B2 (en) * 2009-11-09 2018-02-06 Toray Industries, Inc. Fiber bundle with pieced part, process for producing same, and process for producing carbon fiber

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1639804A (en) * 2002-02-25 2005-07-13 皇家飞利浦电子股份有限公司 Conductive fiber
CN101049991A (en) * 2007-05-09 2007-10-10 山东大学 Method for preparing bush of Nano TiO2 fiber
JP2010133074A (en) * 2008-11-10 2010-06-17 Toray Ind Inc Fiber pieced part and method for producing carbon fiber having the pieced part
JP2010255168A (en) * 2009-03-31 2010-11-11 Toray Ind Inc Process for producing carbon fiber
JP2015120582A (en) * 2013-12-24 2015-07-02 東邦テナックス株式会社 Connection method for fiber yarn, and manufacturing method for carbon fiber
CN208201201U (en) * 2018-05-22 2018-12-07 浙江精功碳纤维有限公司 A kind of carbon fiber continuous production wears the device that furnace connects silk
CN110387602A (en) * 2019-08-16 2019-10-29 广州赛奥碳纤维技术有限公司 A kind of the pre-oxidation equipment and silk head connection method of polyacrylonitrile fibril silk head
CN212560549U (en) * 2020-03-27 2021-02-19 华祥(中国)高纤有限公司 Polyester yarn end-to-end connecting device

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Address after: 132000 No. 117, Kunlun Street, Jilin economic and Technological Development Zone, Jilin City, Jilin Province

Patentee after: Jilin Guoxin Carbon Fiber Co.,Ltd.

Country or region after: China

Address before: 132000 No. 117, Kunlun Street, Jilin economic and Technological Development Zone, Jilin City, Jilin Province

Patentee before: Jilin Baojing carbon material Co.,Ltd.

Country or region before: China