CN114606603A - Carbon fiber and continuous preparation method of carbon fiber - Google Patents
Carbon fiber and continuous preparation method of carbon fiber Download PDFInfo
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- CN114606603A CN114606603A CN202210234392.2A CN202210234392A CN114606603A CN 114606603 A CN114606603 A CN 114606603A CN 202210234392 A CN202210234392 A CN 202210234392A CN 114606603 A CN114606603 A CN 114606603A
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- twisting
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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
Abstract
The invention relates to the field of carbon fibers, and discloses a carbon fiber and a continuous preparation method of the carbon fiber, wherein the continuous preparation method of the carbon fiber comprises the following steps: conducting yarn guiding on the multi-cylinder raw silk bundle, and then conducting carbonization treatment to obtain carbon fibers; wherein the guidewire comprises: when two adjacent front and back raw tows are connected, the tail end of the former raw tow is connected with the head of the latter raw tow through twisting treatment, so that the carbonization treatment can be continuously carried out on a plurality of raw tows. The precursor is connected by twisting, so that continuous preparation of the precursor is realized, the broken rate of the joint is greatly reduced, and the product yield is improved. The carbon fiber product prepared by the preparation method has good quality consistency.
Description
Technical Field
The invention relates to the field of carbon fibers, in particular to a carbon fiber and a continuous preparation method of the carbon fiber.
Background
The carbon fiber has excellent performances of high specific strength, high specific modulus, ablation resistance, wear resistance, fatigue resistance and the like. The carbon fiber can be used as a structural material for bearing load and can also be used as a functional material for playing a role, so the carbon fiber is recommended to be the first of three high-performance fibers. As a reinforcing fiber for advanced composite materials, it has been used in a large amount in the aerospace field such as satellites, launch vehicles, tactical missiles, airplanes and the like. Meanwhile, the method is continuously developed in civilian fields such as cultural and sports, traffic, machinery, buildings and the like.
In the production process of carbon fiber, batch production is generally adopted, several hundreds of raw filaments are arranged on a yarn guide frame, each yarn bundle keeps a certain distance after passing through a tensioner, and horizontally enters a plurality of oxidation furnaces, low-temperature carbonization furnaces and high-temperature carbonization furnaces which are connected in series, and the carbon fiber is obtained through a series of processes such as electrolysis, washing, sizing, coiling and the like. In the production process, after the carbonization of the precursor of the next batch on the guide wire frame is finished, the manual guide wire is needed to be carried out again after the temperature of the oxidation furnace and the carbonization furnace is reduced, and then the carbonization process of the precursor of the next batch is started. In the process, waste silk generated by heating and cooling of the precursor silk guide wire, the oxidation furnace and the carbonization furnace can reduce the yield of the carbon fiber, generally the waste silk accounts for 3-7% of the total yield of the carbon fiber, and the loss is huge.
In the prior art, finished carbon fibers or other high-temperature resistant fibers are adopted to be jointed at the ends of two precursor fibers, so that the production is continuous, for example, in CN208201201U, a carbon fiber knotting mode is adopted to connect the precursor fibers. However, because the difference between the heat conductivity of the carbon fiber or other high-temperature resistant fibers and the heat conductivity of the precursor is too large, the temperature rise rate in an oxidation furnace or a carbonization furnace is very large, and local hot spots are easily caused, so that the joint is broken or loosened, once the joint is broken or loosened, the connection cannot be carried out in the carbonization process, the precursor position on the yarn guide frame cannot be utilized until next shutdown, the energy waste is caused, and the yield is greatly reduced.
Disclosure of Invention
The invention aims to solve the problems that carbon fiber is difficult to produce continuously, the joint breakage rate is high and the product yield is low in the prior art, and provides a carbon fiber and a carbon fiber continuous preparation method.
In order to achieve the above object, an aspect of the present invention provides a method for continuously preparing carbon fibers, comprising: conducting yarn guiding on the multi-cylinder raw silk bundle, and then conducting carbonization treatment to obtain carbon fibers;
wherein the guidewire comprises: when two adjacent front and back raw tows are connected, the tail end of the former raw tow is connected with the head of the latter raw tow through twisting treatment, so that the carbonization treatment can be continuously carried out on a plurality of raw tows.
The second aspect of the present invention provides a carbon fiber produced by the above production method.
According to the technical scheme, the multi-cylinder precursor is continuously fed in a precursor twisting mode, so that the continuous preparation of the carbon fiber is realized. By adopting the twisting mode, local hot spots caused by introducing other fibers or mechanical knotting are reduced, the broken yarn rate of the joint is greatly reduced, and the product yield is improved. The carbon fiber product prepared by the preparation method has good quality consistency.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a method for continuously preparing carbon fibers, which comprises the following steps: conducting yarn guiding on the multi-cylinder raw silk bundle, and then conducting carbonization treatment to obtain carbon fibers;
wherein the guidewire comprises: when two adjacent front and back raw tows are connected, the tail end of the former raw tow is connected with the head of the latter raw tow through twisting treatment, so that the carbonization treatment can be continuously carried out on a plurality of raw tows.
As can be understood by those skilled in the art, in the conventional carbon fiber production process, after the carbonization of the precursor in the previous tube at the same position on the yarn guide frame is finished, the temperature of the oxidation furnace and the carbonization furnace needs to be reduced, the yarn guide is manually pulled, and then the carbonization process of the precursor in the next tube is started. Under the condition, the raw silk at the same position point on the silk guide frame is difficult to realize continuous feeding, and waste silk is generated in the process of heating and cooling the furnace body, so that the production cost is increased. The invention adopts a twisting mode to joint the protofilaments at the same position, changes carbonization from intermittent production to continuous production, and ensures that the joint has low breakage rate at the joint in the carbonization process by twisting, thereby improving the product yield.
In the invention, the twisting treatment can be carried out at any time in the process of guiding the raw silk bundle in the previous cylinder, and can be adjusted according to the actual production process and the requirement. Preferably, after the tail end of the former tube of raw silk bundle starts to guide silk and before carbonization treatment, the tail end of the former tube of raw silk bundle is connected with the head of the latter tube of raw silk bundle by twisting. With the preferred embodiment described above, it is possible to continuously perform the carbonization treatment on a bundle of raw filaments.
According to a preferred embodiment of the present invention, the twisting process comprises: and connecting the tail end of the former raw silk bundle with the head of the latter raw silk bundle to form a twisting connecting section. It will be appreciated that the twisted connecting piece enters the carbonisation process with the previous bundle of raw filaments.
According to a preferred embodiment of the invention, the twisted connecting piece has a length of not more than 10m, preferably 0.01 to 5m, more preferably 0.03 to 1 m. The overlong length of the twisting connecting section can increase the overlapping position points among the protofilaments, the local strength is reduced in the subsequent carbonization treatment process, and the insufficient cohesive force among the protofilaments can be caused if the twisting connecting section is too short, so that the tension among the tension machines is difficult to overcome.
According to the present invention, the specific conditions of the twisting process may be adjusted according to the actual production conditions, and preferably, the conditions of the twisting process include: the twist number is 10 to 500 twists/m, more preferably 15 to 200 twists/m, and still more preferably 30 to 150 twists/m; the twist angle is less than 90 °, preferably 10 to 60 °, and more preferably 20 to 60 °. Three parameters of the length, the twist and the twist angle of the twisting connecting section are properly selected, so that the carbon fiber can be carded and passed through the whole carbon fiber processing process under the action of a tension machine. In the twisting connecting section, because the two strands of protofilaments are cohered, the carbonized quality of the twisted connecting section is different from that of the single strand of protofilaments, the quality of the cohered part is reduced, and the longer the cohered part is, the more the quality is reduced. Too much twist and too large twist angle will cause too large deformation of the original filaments of the cohesive portion and also cause much quality reduction of the cohesive portion.
According to a preferred embodiment of the invention, the strength of the twisted connecting piece is 90 to 100% of the strength of the strand, preferably 95 to 99.99% of the strength of the strand. When the strength of the twisted connecting section reaches 100%, hot spots are more easily generated during the carbonization heat treatment, thereby leading to an increase in the rate of breakage, and when the strength of the twisted connecting section is less than 90%, loosening may occur during the carbonization, which is also disadvantageous for continuous carbonization. It is understood that in the present invention, the conditions of the twisting process affect the strength of the twisted coupling segments.
In the present invention, the strength of the twisted connecting section or the strength of the bundle of raw filaments is tested using the test method specified in GB/T14344-2008.
In the present invention, the twisting process may be performed in a conventional twisting manner as long as the strength range of the twisted coupling segment described above can be satisfied. Preferably, the twisting treatment is air twisting and/or mechanical twisting, and further preferably air twisting. By adopting the preferred embodiment, the yarn breakage rate is reduced, and the product yield is further improved.
According to a preferred embodiment of the present invention, the tow of raw tow is viscose tow and/or polyacrylonitrile tow.
In the present invention, the number of fibers in the bundle is not particularly limited, and the present invention can be applied to a bundle of conventional filaments used in industrial production. Preferably, the number of the fibers in the bundle is 3000-48000, and more preferably 3000-12000. In the above preferred case, twisting by the twisting machine is facilitated.
According to a preferred embodiment of the invention, the speed of travel of the bundle of filaments in the process is between 3 and 10m/min, preferably between 5 and 9 m/min.
According to the invention, the carbonization treatment can be carried out in a conventional manner in the art, and preferably comprises the following steps in sequence: pre-oxidation, low-temperature carbonization and high-temperature carbonization.
According to a preferred embodiment of the present invention, the carbonization process further comprises applying a tension to the bundle of filaments; preferably, the tension is 2 to 6kg, more preferably 2.5 to 3 kg. With the preferred embodiment described above, intermolecular cyclization is facilitated, and the lamellar structure is formed during pre-oxidation, low-temperature carbonization, and high-temperature carbonization.
According to a preferred embodiment of the present invention, wherein the pre-oxidation temperature is 200-350 ℃, preferably 200-300 ℃; the pre-oxidation time is 50-100min, preferably 60-90 min.
According to a preferred embodiment of the invention, the temperature of the low-temperature carbonization is 300-1000 ℃, and the time is 2-10 min; the temperature of the high-temperature carbonization is 800-1500 ℃, and the time is 2-10 min. Preferably, the temperature of the low-temperature carbonization is 300-900 ℃, and the time is 3-8 min; the temperature of the high-temperature carbonization is 1000-1500 ℃, and the time is 3-8 min.
According to a preferred embodiment of the present invention, the method further comprises electrolyzing, washing with water, sizing, and reeling the carbonized precursor filaments. The post-treatment may be carried out in a conventional manner in the art, and is not particularly limited in the present invention.
In another aspect, the invention provides the carbon fiber prepared by the preparation method.
According to the invention, the preparation method avoids the damage to the reaction environment condition caused by furnace shutdown and temperature rise, is beneficial to improving the quality of carbon fiber products, and ensures the consistency.
The present invention will be described in detail below by way of examples.
In the following examples 12K and 24K refer to the number of fibers of the bundle of raw filaments as 12000 and 24000, respectively.
The overall yields of carbon fibers in the following examples and comparative examples are represented by the following proportional relationship:
(precursor quality: carbon fiber yield),
it is understood that the higher the required precursor mass, the lower the overall yield of carbon fibers, which is the mass of precursor required to produce a unit mass of carbon fibers.
Example 1
Adopting 12K polyacrylonitrile fiber bundle protofilament, wherein each protofilament is 60kg, the protofilament on a filament guide frame is 330 tubes, the protofilament keeps a certain distance between the tows after passing through a tension machine (the tension is 3kg), the running speed is 7m/min, each temperature zone is pre-oxidized step by step at the temperature of 220-300 ℃, and the total time is 80 min; and after passing through a tension machine, the pre-oxidized fiber is sequentially carbonized at the low temperature of 350-plus-900 ℃ for 2.8min and at the high temperature of 1100-plus-1500 ℃ for 2.8min, enters an electrolysis device through the tension machine, is sized after being washed by water, and is dried and coiled into carbon fiber. When each precursor is close to an empty cylinder, air twisting is adopted for jointing, the length of a twisting connecting section is 1m, the twist is 20 twists/m, the twist angle is 20 degrees, the strength of the twisting connecting section is 96 percent of the strength of the precursor bundle, the carbonization process is kept to be continuously carried out, the operation period is 37.5 days, each precursor position of a yarn guide frame is jointed for 9 times, each position is carbonized for 10 precursors, and the overall accounting yield is 2.28: 1, the whole production process keeps continuous production, the yield is obviously improved, and the wire breakage rate of a joint is less than 1 percent.
Comparative example 1
According to the method of example 1, the difference is that the twisting and yarn splicing are not carried out, namely, after the carbonization of the raw yarn on the yarn guide frame is finished, the temperature of the oxidation furnace and the carbonization furnace is reduced, the manual yarn guide is carried out again, and the carbonization process of the raw yarn of the next batch is started again. The overall check yield was 2.4: 1.
example 2
Adopting 12K polyacrylonitrile fiber bundle protofilament, wherein each protofilament is 60kg, the protofilament on a silk guide frame is 330, the protofilament keeps a certain distance among the tows after passing through a tension machine (the tension is 2.8kg), the running speed is 7m/min, and the pre-oxidation is carried out for 80min at the temperature of 300 ℃ of 220-; and after passing through a tension machine, the pre-oxidized fiber is sequentially carbonized at the low temperature of 350-plus-900 ℃ for 2.8min and at the high temperature of 1100-plus-1500 ℃ for 2.8min, enters an electrolysis device through the tension machine, is sized after being washed by water, and is dried and coiled into carbon fiber. When each precursor is close to an empty cylinder, mechanical rotation twisting is adopted for jointing, the length of a twisted connecting section is 1m, the twist is 20 twist/m, the twist angle is 20 degrees, the strength of the twisted connecting section is 96.5 percent of the strength of the precursor filament bundle, the carbonization process is kept to be continuously carried out, the operation period is 37.5 days, each precursor position of a filament guide frame is jointed for 9 times, each position is carbonized for 10 precursors, and the overall accounting yield is 2.3: 1, the whole production process keeps continuous production, but the phenomenon of the original connector breaking is more, and the connector breaking rate is less than 1%.
Example 3
Adopting 24K polyacrylonitrile fiber bundle precursor, wherein each precursor is 120kg, the precursor on a silk guide frame is 330, the precursor keeps a certain distance between tows after passing through a tension machine (the tension is 3kg), the running speed is 7m/min, and the precursor is pre-oxidized for 85min at the temperature of 200 plus materials and 300 ℃; and after passing through a tension machine, the pre-oxidized fiber is sequentially carbonized at the low temperature of 900 ℃ for 3min at 300-. Adopt air twisting splicer to splice when every section of thick bamboo precursor is close to empty section of thick bamboo, twist connecting segment length 1m, the twist is 50 twists/m, the angle of twist 20, and twist connecting segment intensity is 98% of precursor beam intensity, keeps the carbonization process to go on in succession, and the cycle of operation 22.5 days, every precursor position of godet frame connects 5 times, 6 precursor of every position carbonization, and whole accounting yield is 2.31: 1, the whole production process keeps continuous production, and the rate of broken filaments of the joint is less than 2 percent.
Example 4
The process of example 1 was followed except that the twist was 50 twists/m, the strength of the twisted connecting portion was 98% of the strength of the strand, and the overall yield was 2.3: 1, the yarn breakage rate of the joint is less than 2 percent.
Example 5
The process of example 1 was followed except that the twist was 200 twists/m, the strength of the twisted connecting piece was 99% of the strength of the raw tow, and the overall yield was 2.32: 1, the yarn breakage rate of the joint is less than 2 percent.
Example 6
The process of example 1 was followed except that the twisted joint length was 0.8m, the twisted joint strength was 96% of the strength of the raw tow, and the overall yield was 2.3: 1, the yarn breakage rate of the joint is less than 2 percent.
Example 7
The process of example 1 was followed except that the twist angle was 10 °, the strength of the twisted connecting piece was 95% of the strength of the raw tow, and the overall yield was 2.32: 1, the yarn breakage rate of the joint is less than 2 percent.
Example 8
The process of example 1 was followed except that the twist angle was 60 °, the strength of the twisted connecting piece was 97% of the strength of the raw tow, and the overall yield was 2.33: 1 percent and the broken wire rate of the joint is less than 3 percent.
Comparative example 2
Following the procedure of example 1 except that the method of example 1 of CN208201201U was used for the grafting, the overall calculated yield was 2.34: 1, the filament breakage rate is less than 4 percent. It can be seen that, because the difference between the thermal conductivity of the carbon fiber or other high temperature resistant fiber and the thermal conductivity of the precursor is too large, the temperature rise rate in the oxidation furnace or carbonization furnace is greatly different, which easily causes the breakage of the joint, thereby causing the yield to decrease.
According to the embodiment and the comparative example, the twisting mode is adopted to connect the precursor, so that the carbonization process is changed from intermittent production to continuous production, the continuous preparation of the carbon fiber is realized, the filament breakage rate is low, and the product yield is high.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including various technical features being combined in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A method for continuously producing carbon fibers, comprising: conducting yarn guiding on the multi-cylinder raw silk bundle, and then conducting carbonization treatment to obtain carbon fibers;
wherein the guidewire comprises: when two adjacent original tows in the front and back are connected, the tail end of the original tow in the front cylinder is connected with the head of the original tow in the back cylinder through twisting treatment, and continuous carbonization treatment of multiple original tows is realized.
2. The production method according to claim 1, wherein the twisting process includes: connecting the tail end of the former raw silk bundle with the head of the latter raw silk bundle to form a twisting connecting section;
preferably, the twisted connecting section has a length of not more than 10m, preferably 0.01 to 5m, and more preferably 0.03 to 1 m.
3. The production method according to claim 1 or 2, wherein the conditions of the twisting process include: the twist number is 10-500 twist/m, preferably 15-200 twist/m; the twist angle is less than 90 °, preferably 10-60 °.
4. The production method according to any one of claims 1 to 3, wherein the strength of the twisted connecting piece is 90 to 100% of the strength of the strand bundle, preferably 95 to 99.99% of the strength of the strand bundle, wherein;
preferably, the twisting treatment is air twisting and/or mechanical twisting, and further preferably air twisting.
5. The production method according to any one of claims 1 to 4, wherein the tow of raw tow is a viscose tow and/or a polyacrylonitrile tow.
6. The method according to any one of claims 1 to 5, wherein the number of fibers in the bundle is 3000-48000, preferably 3000-12000.
7. The production method according to any one of claims 1 to 6, wherein the running speed of the bundle of raw filaments in the method is 3 to 10 m/min.
8. The production method according to any one of claims 1 to 7, wherein the carbonization treatment sequentially comprises: pre-oxidation, low-temperature carbonization and high-temperature carbonization;
preferably, the carbonization treatment further comprises applying tension to the bundle of raw filaments;
preferably, the tension is 2 to 6kg, more preferably 2.5 to 3 kg.
9. The preparation method according to claim 8, wherein the pre-oxidation temperature is 200-350 ℃, preferably 200-300 ℃; the pre-oxidation time is 50-100min, preferably 60-90 min;
preferably, the temperature of the low-temperature carbonization is 300-1000 ℃, and the time is 2-10 min; the temperature of the high-temperature carbonization is 800-1500 ℃, and the time is 2-10 min;
preferably, the preparation method further comprises the steps of electrolyzing, washing, sizing and reeling the carbonized precursor fiber.
10. A carbon fiber produced by the production method according to any one of claims 1 to 9.
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| JPS58208420A (en) * | 1982-05-26 | 1983-12-05 | Toray Ind Inc | Continuous production of carbon fiber |
| US4466949A (en) * | 1981-09-16 | 1984-08-21 | Toray Industries, Inc. | Process for continuously producing carbon fibers |
| JPH10226918A (en) * | 1997-02-14 | 1998-08-25 | Toray Ind Inc | Carbon fiber, and its production and production apparatus |
| JP2002302341A (en) * | 2001-04-09 | 2002-10-18 | Mitsubishi Rayon Co Ltd | Ending machine and carbon fiber producing method |
| JP2008190068A (en) * | 2007-02-02 | 2008-08-21 | Mitsubishi Rayon Co Ltd | Method for producing yarn of carbon fiber bundle |
| CN107385531A (en) * | 2017-06-21 | 2017-11-24 | 兰州蓝星纤维有限公司 | A kind of processing method of big tow precursor joint |
| CN211546739U (en) * | 2019-11-13 | 2020-09-22 | 广州赛奥碳纤维技术有限公司 | Polyacrylonitrile pre-oxidized fiber head connects silk device |
-
2022
- 2022-03-10 CN CN202210234392.2A patent/CN114606603A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4466949A (en) * | 1981-09-16 | 1984-08-21 | Toray Industries, Inc. | Process for continuously producing carbon fibers |
| JPS58208420A (en) * | 1982-05-26 | 1983-12-05 | Toray Ind Inc | Continuous production of carbon fiber |
| JPH10226918A (en) * | 1997-02-14 | 1998-08-25 | Toray Ind Inc | Carbon fiber, and its production and production apparatus |
| JP2002302341A (en) * | 2001-04-09 | 2002-10-18 | Mitsubishi Rayon Co Ltd | Ending machine and carbon fiber producing method |
| JP2008190068A (en) * | 2007-02-02 | 2008-08-21 | Mitsubishi Rayon Co Ltd | Method for producing yarn of carbon fiber bundle |
| CN107385531A (en) * | 2017-06-21 | 2017-11-24 | 兰州蓝星纤维有限公司 | A kind of processing method of big tow precursor joint |
| CN211546739U (en) * | 2019-11-13 | 2020-09-22 | 广州赛奥碳纤维技术有限公司 | Polyacrylonitrile pre-oxidized fiber head connects silk device |
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