CN109402794A - Weaken the equipment and heat treatment method of skin-core structure in carbon fiber - Google Patents
Weaken the equipment and heat treatment method of skin-core structure in carbon fiber Download PDFInfo
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- CN109402794A CN109402794A CN201710699349.2A CN201710699349A CN109402794A CN 109402794 A CN109402794 A CN 109402794A CN 201710699349 A CN201710699349 A CN 201710699349A CN 109402794 A CN109402794 A CN 109402794A
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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
- 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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Abstract
The present invention relates to the equipment and heat treatment technics of skin-core structure in a kind of decrease carbon fiber, it is serious mainly to solve preoxidized fiber skin-core structure in existing carbon fiber preparation process, compactness difference and the big problem of line density coefficient of dispersion, equipment by using skin-core structure in carbon fiber fiber is weakened, including at least No.1 oxidation furnace (1), No. two oxidation furnaces (2), No. three oxidation furnaces (3), (4) four oxidation furnaces of No. four oxidation furnaces, wherein, the oxidation furnace all uses electrical heating type tube type drying furnace, inside is stainless steel burner hearth, nichrome wire is wound on burner hearth, heater strip (9) winding density on each oxidation furnace burner hearth (8), it is increasing along wire direction, so that the temperature of each oxidation furnace import to outlet can realize the technical solution of 10~50 DEG C of temperature difference, preferably solves problem above, it can be used for In the industrial production of carbon fiber.
Description
Technical field
The present invention relates to the equipment and heat treatment method of skin-core structure in a kind of decrease carbon fiber.
Technical background
Carbon fiber is fibrous polymer of the phosphorus content made of being changed as organic fiber through solid phase reaction 90% or more.
It has high specific strength, high ratio modulus, high temperature resistant, resistant to chemical etching, endurance, heat shock resistance, anti-radiation and specific gravity small etc. by one
Serial excellent properties belong to typical high-performance fiber.Foreign countries have been realized in commercially producing for high-strength carbon fiber, and I
State is also in development and trial production stage, while beauty, Deng developed country take technology blockage to my family, seriously constrain me
The development of state's national defence related fields.Therefore, the research work of high-strength carbon fibre has been increasingly subject to pay attention to.
The preparation process of carbon fiber includes polymerization, spinning, pre-oxidation and carbonization, and wherein preoxidation process is carbon fiber preparation
Committed step in the process, the quality of preoxidized fiber directly determine the mechanical property of final carbon fiber.In preoxidation process
Oxygen is from outward appearance to inner essence spread to fibrous inside, with the progress of pre-oxidation, forms fine and close ladder on the surface layer of fiber first
Shape structured thin layers hinder oxygen inwardly to spread, and so that fiber core is formed the sandwich layer of cyclisation, degree of cross linking angle, here it is skin-core structures.
Skin-core structure be cause the mechanical properties such as carbon fiber strength reduce the main reason for one of.Therefore, in recent years scientists in depth
Enter the elimination how research just focuses on skin-core structure since polymerization spinning, pre-oxidizing stage, it is uniformly equal to produce external and internal compositions
Matter oxidization fiber.Producing homogeneous oxidization fiber is current one of the Major Technology for improving carbon fiber performance, domestic scientific research mechanism and
Manufacturing enterprise generally takes four or six pre-oxidation furnaces, since there are temperature gradients between each pre-oxidation furnace, so that preoxidized fiber
The having a certain difference property of chemical structure of skin zone and core.Skin-core structure is further inherited and is developed in carbonisation,
A kind of fault of construction is evolved into, the structure and performance of final carbon fiber are influenced.
" preparation method of polyacrylonitrile-based carbon fiber precursor without skin-core structure " (patent No. that ten thousand actinium persons of outstanding talent et al. deliver
CN201110008396.0 a kind of polyacrylonitrile-based carbon fiber precursor without skin-core structure of carbon fibre precursor technical field) is described
Preparation method, it is heated molten by the way that polyacrylonitrile resin is added in water or alcohol compound and organic solvent after mixing
Polyacrylonitrile spinning solution is obtained by filtration after swollen dissolution process；It will spray after polyacrylonitrile spinning solution maturation process and obtained after squeezing again
Above-mentioned nascent precursor is successively carried out washing stretching by nascent precursor, second level hot water stretches, compacting by drying and saturated vapor are drawn
It stretches, obtains polyacrylonitrile base carbon fiber precursors.Large-scale production can be carried out on existing industrialization spinning equipment, prepare nothing
The high-quality polyacrylonitrile base carbon fiber precursors that skin-core structure, defect are few, fiber number is small, intensity is high, and production can be effectively reduced
Cost；" influence factor and prevention and control measure of PAN-based stabilized fiber skin-core structure " (" plastics industry " that Yu Meijie et al. is delivered
6th phase (41) in 2010 volume, p1019-1022) in describe under constant temperature and gradient increased temperature both of which, to different fiber numbers, cross
3 kinds of polyacrylonitrile fibrils of cross sectional shape have carried out pre-oxidation treatment, using scanning electron microscope, optical microscopy, elemental analysis etc.
The technical research skin-core structure of oxidization fiber and the diffusion of oxygen element the result shows that, for constant temperature mode, in 250 DEG C of heating 1h
Oxidization fiber produced apparent skin-core structure, and for gradient increased temperature mode, just start core-skin knot occur until 275 DEG C
Structure；The cross-sectional shape of precursor does not influence the diffusion of oxygen, under identical heating condition, the skin thickness of kidney shaped cross section oxidization fiber with
Circular cross-section it is identical；Precursor fiber number is smaller, is more easy to get the fine-denier and gradient appropriate of the oxidization fiber precursor of homogeneous
The pre-oxidation process that heats up is the important guarantee for obtaining high-quality oxidization fiber.
Although part researcher has done part to the formation mechenism of skin-core structure and studied, there is no propose to weaken
The equipment and specific method of skin-core structure.The present invention proposes a kind of effectively decrease carbon fiber from the angle of equipment and technique
Tie up the equipment and heat treatment method of skin-core structure.
Summary of the invention
The first technical problem to be solved by the present invention is that skin-core structure is serious, fine and close in existing carbon fiber preoxidation process
Property the difference and big problem of line density coefficient of dispersion, a kind of equipment of skin-core structure in decrease carbon fiber is provided.The equipment is for gathering
In the preparation process of acrylonitrile base carbon fiber, has and weaken preoxidized fiber skin-core structure, reduce the discrete system of preoxidized fiber line density
Several advantages.
The second technical problem to be solved by the present invention is that skin-core structure is serious in existing carbon fiber preoxidation process, causes
Close property difference and the big problem of line density coefficient of dispersion, by using solving core-skin in decrease carbon fiber described in one of technical problem
The equipment of structure, provides a kind of heat treatment method for weakening skin-core structure in carbon fiber, and this method is used for polyacrylonitrile-radical carbon fiber
In the preparation process of dimension, has the advantages that weaken preoxidized fiber skin-core structure, reduces preoxidized fiber line density coefficient of dispersion.
In order to solve one of technical problem, the technical solution adopted by the present invention are as follows: core-skin in a kind of decrease carbon fiber fiber
The equipment of structure, including at least oxidation furnace 2, three of No.1 oxidation furnace 1, two oxidation furnace 3, No. four oxidation furnaces, 4 four oxidation furnaces,
Wherein, the oxidation furnace all uses electrical heating type tube type drying furnace, and inside is burner hearth, winds heater strip, each oxygen on burner hearth
9 winding density of heater strip changed on furnace burner hearth 8 is different, and along wire direction, winding density is increasing, so that each oxidation furnace
The temperature of import to outlet can realize 10~50 DEG C of temperature difference.
In above-mentioned technical proposal, the heater strip is preferably nichrome wire, and the burner hearth is preferably stainless steel burner hearth.
In above-mentioned technical proposal, it is also preferable to include driving stations 7 for the equipment, for carrying out necessary drawing-off to fiber；Institute
State the blowing device being preferably provided in oxidation furnace along wire direction；The equipment preferably includes six oxidation furnaces, wherein each oxygen
The blowing device changed in furnace is dried along wire direction level；The blowing device of No.1 oxidation furnace 1 as shown in Figure 1 is preferably along wire side
To from the right side turn left blowing, No. two oxidation furnaces 2 blowing device preferably dry from left to right along wire direction, No. three oxidation furnaces 3
Blowing device preferably along wire direction from the right side turn left blowing, No. four oxidation furnaces 4 blowing device preferably along wire direction it is past from the right side
Zuo Feng, No. five oxidation furnaces 5 blowing device preferably dry from left to right along wire direction, the blowing device of No. six oxidation furnaces 6 it is excellent
Choosing is dried from left to right along wire direction；Air of the blowing preferably after the pre-heat treatment in the oxidation furnace.
In above-mentioned technical proposal, the temperature of the oxidation furnace is preferably the inlet temperature of the latter oxidation furnace equal to previous
The outlet temperature of oxidation furnace can preferably reduce skin-core structure.
In above-mentioned technical proposal, the equipment can also include thread supplying machine, low-temperature carbonization furnace, high temperature carbonization furnace, at surface
Reason and starching drying device, receive silk machine.
In order to solve the two of technical problem, a kind of the technical solution adopted by the present invention are as follows: core-skin in decrease carbon fiber fiber
The heat treatment method of structure, using any equipment in technical solution described in one of technical problem is solved, successively by with
Lower step: precursor is after thread supplying machine uncoiling, by six oxidation furnaces, low temperature carbonization furnace, high temperature carbonization furnace, surface treatment and starching
Dry, finally winding obtains carbon fiber；It is characterized in that 1 temperature of No.1 pre-oxidation furnace is between 160-210 DEG C, and from inlet temperature
Consecutive variations are to outlet temperature；No. two 2 temperature of pre-oxidation furnace are between 185-235 DEG C, and from inlet temperature consecutive variations to outlet
Temperature DEG C；No. three 3 temperature of pre-oxidation furnace are between 200-245 DEG C, and from inlet temperature consecutive variations to outlet temperature；No. four pre- oxygen
4 temperature of furnace is between 215-260 DEG C, and from inlet temperature consecutive variations to outlet temperature；No. five 5 temperature of pre-oxidation furnace are in 230-
Between 265 DEG C, and from inlet temperature consecutive variations to outlet temperature；No. six 6 temperature of pre-oxidation furnace between 240-270 DEG C, and from
Inlet temperature consecutive variations are to outlet temperature；Meanwhile the inlet temperature of the same oxidation furnace is less than outlet temperature.
In above-mentioned technical proposal, the temperature of the oxidation furnace is preferably the inlet temperature of the latter oxidation furnace equal to previous
The outlet temperature of oxidation furnace；The No.1 oxidation furnace and No. two oxidation furnaces are preferably low-temperature space, No. three oxidation furnaces and No. four oxidations
Furnace is preferably middle warm area, and No. five oxidation furnaces and No. six oxidation furnaces are preferably high-temperature region；It is preferred that applying positive drawing-off in low-temperature space, preferably
Apply zero drawing-off in middle warm area, preferably applies negative drawing-off in high-temperature region；The degree of draft of the low-temperature space is 1~8%, the medium temperature
The degree of draft in area is 0%, and the degree of draft of the high-temperature region is -2~-5%；Fiber after oxidation furnace is heat-treated is preferably described
300~800 DEG C of low-temperature carbonization under inert atmosphere in low temperature carbonization furnace, then in the high temperature carbonization furnace under inert atmosphere
900-1400 DEG C of high temperature carbonization.
The equipment that the above method uses is continous way pre-oxidation furnace-low temperature carbonization furnace-high temperature carbonization furnace, wherein the pre- oxygen of continous way
Furnace is heated up using six segmentations, and wherein No.1 pre-oxidation furnace temperature is between 180-195 DEG C, and No. two pre-oxidation furnace temperature are at 195-210 DEG C
Between, No. three pre-oxidation furnace temperature are between 210-235 DEG C, and No. four pre-oxidation furnace temperature are between 235-245 DEG C, No. five pre-oxidation furnace temperature
Degree is between 245-255 DEG C, and No. six pre-oxidation furnace temperature are between 255-265 DEG C.
The present invention does not change polymerization spinning and carbonization technique, passes through in the preparation process of polyacrylonitrile-based carbon fibre
Oxidation furnace all uses continous way heating method, by the winding density of change pre-oxidation furnace surface of burner hearth nichrome resistance wire, respectively
The power and throughput of hot spot will be pre-oxidized entirely so that temperature is distributed along fiber orientation in continuous increase in pre-oxidation furnace
Temperature gradient is reduced to minimum in the process, pre- only by changing under conditions of not changing polymerization spinning and carbonization technique
Temperature is gentle in oxidation process flows away to the skin-core structure that can weaken preoxidized fiber with flow, to prepare high performance carbon fiber
Dimension lays the foundation.
Preoxidized fiber obtained is carried out to the test of skin-core structure, test method is as follows: being sliced using epoxy resin embedding
Method, amplifies 1000 times of skin-core structures observed and measure fiber under an optical microscope, and each sample surveys 50 monofilament cross
The outer diameter and core diameters in section, and take its average value.
Shoe designing (FS%) measure equation:
Using technical solution of the present invention, continous way heating method is all used by oxidation furnace, by changing pre-oxidation furnace furnace
The power and throughput of the winding density of thorax surface nickel chromium alloy resistive silk, each hot spot, so that temperature is along fine in pre-oxidation furnace
Dimension trend increases distribution in continuous, and carbon fiber shoe designing obtained is 90% or more, achieves preferable technical effect.
Below by embodiment, the present invention is further elaborated:
Detailed description of the invention
Fig. 1 is the pre-oxidation process of skin-core structure in decrease carbon fiber of the present invention, and carbon fibre precursor is after pre-treatment
Sequentially enter No. 1 oxidation furnace, No. 2 oxidation furnaces, No. 3 oxidation furnaces, No. 4 oxidation furnaces, No. 5 oxidation furnaces and No. 6 oxidation furnaces, each oxidation
Mode of drying in furnace is horizontal blowing, and wind direction is identical as wire direction.
Fig. 2 is the equipment structure chart of pre-oxidation furnace.
Fig. 3 is the skin-core structure of carbon fibers schematic diagram that shoe designing test method refers to.
In Fig. 1,1 is No. 1 oxidation furnace, and 2 be No. 2 oxidation furnaces, and 3 be No. 3 oxidation furnaces, and 4 be No. 4 oxidation furnaces, and 5 be No. 5 oxidations
Furnace, 6 be No. 6 oxidation furnaces, and 7 be draw roll.
In Fig. 2,8 be oxidation furnace burner hearth, 9 nichrome wires wound for oxidation furnace tube skin.
In Fig. 3, Rs is fibre section radius, and Rc is fiber core radius.
The present invention will be further described below by way of examples, but is not limited only to the present embodiment.
Specific embodiment
[embodiment 1]
Polyacrylonitrile fibril is pre-oxidized in six segmentation pre-oxidation furnaces, heat treatment process is as shown in Figure 1.Pass through adjusting
The power of each hot spot in each pre-oxidation furnace, so that temperature gradually rises along fiber direction of travel in each pre-oxidation furnace, each oxidation furnace
Middle blowing mode all takes horizontal blowing, and wind direction is consistent with wire direction.Wherein No. 1 pre-oxidation furnace temperature 175-190 DEG C it
Between gradually rise；No. 2 pre-oxidation furnace temperature gradually rise between 190-210 DEG C, and No. 3 pre-oxidation furnace temperature are between 210-225 DEG C
Gradually rise, No. 4 pre-oxidation furnace temperature gradually rise between 225-240 DEG C, No. 5 pre-oxidation furnace temperature between 240-255 DEG C by
Edge up height, and No. 6 pre-oxidation furnace temperature gradually rise between 255-270 DEG C.Preoxidized fiber obtained is carried out to the survey of skin-core structure
Examination, test result are shown in Table 1.
[embodiment 2]
Polyacrylonitrile fibril is pre-oxidized in six segmentation pre-oxidation furnaces, heat treatment process is as shown in Figure 1.Pass through adjusting
The power of each hot spot in each pre-oxidation furnace, so that temperature gradually rises along fiber direction of travel in each pre-oxidation furnace, each oxidation furnace
Middle blowing mode all takes horizontal blowing, and wind direction is consistent with wire direction.Wherein No. 1 pre-oxidation furnace temperature 175-195 DEG C it
Between gradually rise；No. 2 pre-oxidation furnace temperature gradually rise between 195-215 DEG C, and No. 3 pre-oxidation furnace temperature are between 215-230 DEG C
Gradually rise, No. 4 pre-oxidation furnace temperature gradually rise between 230-245 DEG C, No. 5 pre-oxidation furnace temperature between 245-260 DEG C by
Edge up height, and No. 6 pre-oxidation furnace temperature gradually rise between 260-270 DEG C.Preoxidized fiber obtained is carried out to the survey of skin-core structure
Examination, test result are shown in Table 1.
[embodiment 3]
Polyacrylonitrile fibril is pre-oxidized in six segmentation pre-oxidation furnaces, heat treatment process is as shown in Figure 1.Pass through adjusting
The power of each hot spot in each pre-oxidation furnace, so that temperature gradually rises along fiber direction of travel in each pre-oxidation furnace, each oxidation furnace
Middle blowing mode all takes horizontal blowing, and wind direction is consistent with wire direction.Wherein No. 1 pre-oxidation furnace temperature 175-185 DEG C it
Between gradually rise；No. 2 pre-oxidation furnace temperature gradually rise between 185-205 DEG C, and No. 3 pre-oxidation furnace temperature are between 205-220 DEG C
Gradually rise, No. 4 pre-oxidation furnace temperature gradually rise between 220-235 DEG C, No. 5 pre-oxidation furnace temperature between 235-250 DEG C by
Edge up height, and No. 6 pre-oxidation furnace temperature gradually rise between 250-265 DEG C.Preoxidized fiber obtained is carried out to the survey of skin-core structure
Examination, test result are shown in Table 1.
[embodiment 4]
Polyacrylonitrile fibril is pre-oxidized in six segmentation pre-oxidation furnaces, heat treatment process is as shown in Figure 1.Pass through adjusting
The power of each hot spot in each pre-oxidation furnace, so that temperature gradually rises along fiber direction of travel in each pre-oxidation furnace, while each oxygen
Change blowing mode in furnace and all take vertical blowing, blowing direction is vertical with wire direction.Wherein No. 1 pre-oxidation furnace temperature is in 175-
It is gradually risen between 190 DEG C；No. 2 pre-oxidation furnace temperature gradually rise between 190-210 DEG C, and No. 3 pre-oxidation furnace temperature are in 210-
It is gradually risen between 225 DEG C, No. 4 pre-oxidation furnace temperature gradually rise between 225-240 DEG C, and No. 5 pre-oxidation furnace temperature are in 240-
It is gradually risen between 255 DEG C, No. 6 pre-oxidation furnace temperature gradually rise between 255-270 DEG C.Preoxidized fiber obtained is carried out
The test of skin-core structure, test result are shown in Table 1.
[embodiment 5]
Polyacrylonitrile fibril is pre-oxidized in six segmentation pre-oxidation furnaces, heat treatment process is as shown in Figure 1.Pass through adjusting
The power of each hot spot in each pre-oxidation furnace, so that temperature gradually rises along fiber direction of travel in each pre-oxidation furnace, while each oxygen
Change blowing mode in furnace and all take horizontal blowing, and wind direction is consistent with wire direction.Wherein No. 1 pre-oxidation furnace temperature is in 175-195
It is gradually risen between DEG C；No. 2 pre-oxidation furnace temperature gradually rise between 190-215 DEG C, and No. 3 pre-oxidation furnace temperature are at 210-230 DEG C
Between gradually rise, No. 4 pre-oxidation furnace temperature gradually rise between 225-245 DEG C, No. 5 pre-oxidation furnace temperature 240-260 DEG C it
Between gradually rise, No. 6 pre-oxidation furnace temperature gradually rise between 255-270 DEG C.Preoxidized fiber obtained is subjected to skin-core structure
Test, test result is shown in Table 1.
[comparative example 1]
Polyacrylonitrile fibril is pre-oxidized in six segmentation pre-oxidation furnaces, heat treatment process is as shown in Figure 1.Pass through adjusting
The power of each hot spot in each pre-oxidation furnace, so that temperature is uniform in each pre-oxidation furnace, along fiber wire direction temperature in each oxidation furnace
Degree uniformity reaches ± 1.5 DEG C, while mode of drying in each oxidation furnace takes horizontal blowing, and wind direction and wire direction one
It causes.Wherein No. 1 pre-oxidation furnace temperature is 180 DEG C；No. 2 pre-oxidation furnace temperature are 210 DEG C, and No. 3 pre-oxidation furnace temperature are 225 DEG C, No. 4 pre- oxygen
Furnace temperature is 240 DEG C, and No. 5 pre-oxidation furnace temperature are 255 DEG C, and No. 6 pre-oxidation furnace temperature are 265 DEG C.Preoxidized fiber obtained is carried out
The test of skin-core structure, test result are shown in Table 1.
[comparative example 2]
Polyacrylonitrile fibril is pre-oxidized in six segmentation pre-oxidation furnaces, heat treatment process is as shown in Figure 1.Pass through adjusting
The power of each hot spot in each pre-oxidation furnace, so that temperature is uniform in each pre-oxidation furnace, along fiber wire direction temperature in each oxidation furnace
Degree uniformity reaches ± 1.5 DEG C, while mode of drying in each oxidation furnace takes vertical blowing, blowing direction and wire direction
Vertically.Wherein No. 1 pre-oxidation furnace temperature is 180 DEG C；No. 2 pre-oxidation furnace temperature are 210 DEG C, and No. 3 pre-oxidation furnace temperature are 225 DEG C, No. 4
Pre-oxidation furnace temperature is 240 DEG C, and No. 5 pre-oxidation furnace temperature are 255 DEG C, and No. 6 pre-oxidation furnace temperature are 265 DEG C.By preoxidized fiber obtained
The test of skin-core structure is carried out, test result is shown in Table 1.
Obviously, using apparatus and method of the present invention, can achieve the purpose for reducing skin-core structure in carbon fiber, have compared with
Big technical advantage, can be used in the industrial production of carbon fiber.
Table 1
| Sample number into spectrum | Shoe designing (%) |
| Embodiment 1 | 96.2 |
| Embodiment 2 | 94.7 |
| Embodiment 3 | 93.6 |
| Embodiment 4 | 85.6 |
| Embodiment 5 | 86.2 |
| Comparative example 1 | 81.6 |
| Comparative example 2 | 84.2 |
Claims (10)
1. it is a kind of weaken carbon fiber fiber in skin-core structure equipment, including at least No.1 oxidation furnace (1), No. two oxidation furnaces (2),
(4) four No. three oxidation furnaces (3), No. four oxidation furnaces oxidation furnaces, wherein the oxidation furnace all uses electrical heating type tube type drying
Furnace, inside are burner hearth, wind heater strip on burner hearth, heater strip (9) winding density on each oxidation furnace burner hearth (8), along walking
Silk direction is increasing, so that the temperature of each oxidation furnace import to outlet can realize 10~50 DEG C of temperature difference.
2. the equipment according to claim 1 for weakening skin-core structure in carbon fiber fiber, it is characterised in that the heater strip
For nichrome wire, the burner hearth is stainless steel burner hearth.
3. the equipment according to claim 1 for weakening skin-core structure in carbon fiber fiber, it is characterised in that the oxidation furnace
The interior blowing device being equipped with along wire direction.
4. the equipment according to claim 3 for weakening skin-core structure in carbon fiber fiber, it is characterised in that the equipment packet
Include six oxidation furnaces, wherein the blowing device in each oxidation furnace is dried along wire direction level.
5. the equipment according to claim 3 or 4 for weakening skin-core structure in carbon fiber fiber, it is characterised in that the oxidation
Blowing in furnace is the air after the pre-heat treatment.
6. a kind of heat treatment method for weakening skin-core structure in carbon fiber fiber, using equipment described in Claims 1 to 5, according to
It is secondary by following steps: precursor is after thread supplying machine uncoiling, at six oxidation furnaces, low temperature carbonization furnace, high temperature carbonization furnace, surface
Reason and starching are dry, and finally winding obtains carbon fiber；It is characterized in that No.1 pre-oxidation furnace (1) temperature is between 160-210 DEG C, and
From inlet temperature consecutive variations to outlet temperature；No. two pre-oxidation furnace (2) temperature connect between 185-235 DEG C, and from inlet temperature
It is continuous to be changed to outlet temperature；No. three pre-oxidation furnace (3) temperature are between 200-245 DEG C, and from inlet temperature consecutive variations to outlet
Temperature；No. four pre-oxidation furnace (4) temperature are between 215-260 DEG C, and from inlet temperature consecutive variations to outlet temperature；No. five pre- oxygen
Furnace (5) temperature is between 230-265 DEG C, and from inlet temperature consecutive variations to outlet temperature；No. six pre-oxidation furnace (6) temperature exist
Between 240-270 DEG C, and from inlet temperature consecutive variations to outlet temperature；Meanwhile the inlet temperature of the same oxidation furnace is less than
Outlet temperature.
7. the heat treatment method according to claim 6 for weakening skin-core structure in carbon fiber fiber, it is characterised in that described
The temperature of oxidation furnace is that the inlet temperature of the latter oxidation furnace is equal to the outlet temperature of previous oxidation furnace.
8. the heat treatment method according to claim 6 for weakening skin-core structure in carbon fiber fiber, it is characterised in that described
No.1 oxidation furnace and No. two oxidation furnaces are low-temperature space, and No. three oxidation furnaces and No. four oxidation furnaces are middle warm area, No. five oxidation furnaces and six
Number oxidation furnace is high-temperature region, and low-temperature space applies positive drawing-off, middle warm area applies zero drawing-off, high-temperature region applies negative drawing-off.
9. the heat treatment method according to claim 8 for weakening skin-core structure in carbon fiber fiber, it is characterised in that described
The degree of draft of low-temperature space is 1~8%, and the degree of draft of the middle warm area is 0%, the degree of draft of the high-temperature region is -2~-5%.
10. the heat treatment method according to claim 6 for weakening skin-core structure in carbon fiber fiber, it is characterised in that through oxygen
Fiber after changing furnace treatment reason 300~800 DEG C of the low-temperature carbonization under inert atmosphere in the low temperature carbonization furnace, then in the height
900-1400 DEG C of high temperature carbonization under inert atmosphere in warm carbide furnace.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110846744A (en) * | 2019-12-18 | 2020-02-28 | 河南永煤碳纤维有限公司 | Method for regulating and controlling homogenization of carbon fiber pre-oxidized fiber and pre-oxidation furnace |
| CN111218733A (en) * | 2020-03-13 | 2020-06-02 | 北京化工大学 | Preparation method of large-diameter high-strength medium-modulus carbon fiber |
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| CN102704043A (en) * | 2012-06-20 | 2012-10-03 | 北京化工大学 | Preparation method of polyacrylonitrile pre-oxidation fiber and carbon fiber |
| CN103352269A (en) * | 2013-06-19 | 2013-10-16 | 合肥日新高温技术有限公司 | Pre-oxidation furnace with air uniformizing structure |
| CN105568432A (en) * | 2014-10-14 | 2016-05-11 | 中国石油化工股份有限公司 | Device and method for producing low-dispersion coefficient carbon fibers |
| CN106480553A (en) * | 2016-10-31 | 2017-03-08 | 哈尔滨天顺化工科技开发有限公司 | A kind of pre-oxidation device for carbon fiber production |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102704043A (en) * | 2012-06-20 | 2012-10-03 | 北京化工大学 | Preparation method of polyacrylonitrile pre-oxidation fiber and carbon fiber |
| CN103352269A (en) * | 2013-06-19 | 2013-10-16 | 合肥日新高温技术有限公司 | Pre-oxidation furnace with air uniformizing structure |
| CN105568432A (en) * | 2014-10-14 | 2016-05-11 | 中国石油化工股份有限公司 | Device and method for producing low-dispersion coefficient carbon fibers |
| CN106480553A (en) * | 2016-10-31 | 2017-03-08 | 哈尔滨天顺化工科技开发有限公司 | A kind of pre-oxidation device for carbon fiber production |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110846744A (en) * | 2019-12-18 | 2020-02-28 | 河南永煤碳纤维有限公司 | Method for regulating and controlling homogenization of carbon fiber pre-oxidized fiber and pre-oxidation furnace |
| CN111218733A (en) * | 2020-03-13 | 2020-06-02 | 北京化工大学 | Preparation method of large-diameter high-strength medium-modulus carbon fiber |
| CN111218733B (en) * | 2020-03-13 | 2021-10-15 | 北京化工大学 | Preparation method of large-diameter high-strength medium-modulus carbon fiber |
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