JPH0627372B2 - Pitch-type carbon fiber centrifugal spinning device - Google Patents

Description

The present invention relates to a pitch-based carbon fiber centrifugal spinning apparatus.

More specifically, the present invention relates to a pitch-based carbon fiber centrifugal spinning apparatus that smoothly spins a raw fiber yarn having excellent properties.

(Background Art and Problems) Conventionally, as a centrifugal spinning device for pitch-based carbon fibers, a centrifugal spinning device in which a rotation axis of a rotary nozzle is vertical and a discharge direction of fibers is horizontal is widely used.

In the case of spinning with a centrifugal spinning device, the spinning is not performed using a stretching device because the spinning is short fibers.

This centrifugal spinning device spins a carbon fiber raw yarn by ejecting a melt pitch from a nozzle opening by a centrifugal force generated by high-speed rotation of a rotary nozzle.

In the process of centrifugally spinning pitch-based carbon fibers, it is important to keep the temperature near the rotary nozzle constant and smooth the air flow around it.

When the temperature near the rotating nozzle drops and falls below a certain temperature, the spun yarn partially ejects as a lump, a so-called ball-splitting phenomenon (shot) occurs, and spinning cannot be performed smoothly or spun. A necking phenomenon occurs in which the yarn diameter becomes uneven in the length direction. Also, when the temperature drops extremely,
The nozzle mouth may be clogged with spun yarn.

Further, if the air around the rotary nozzle does not flow smoothly, a necking phenomenon in which the yarn diameter of the spun yarn becomes uneven in the length direction due to slack in the middle due to a decrease in the flow velocity of the air, turbulence, or the like becomes prominent.

Even if the carbon fiber raw yarn in which the necking phenomenon has occurred is infusibilized and carbonized, high-strength carbon fibers cannot be obtained.

Conventionally, the control of the air flow in the spinning process is insufficient, and moreover, if the amount of air blown in is increased in order not to reduce the flow velocity of the air, turbulence in the air flow easily occurs, so that the occurrence of necking phenomenon occurs. It was difficult to prevent.

Therefore, it has been desired to develop a technique for sufficiently controlling the temperature and the air flow around the rotary nozzle to prevent the necking phenomenon from occurring.

Methods for smoothing the flow of air as a means for conveying spun yarn include, for example, JP-A-59-150106 and JP-A-60-167908.

In Japanese Patent Laid-Open No. 59-150106, upper and lower "guide plates" are installed horizontally around the rotary nozzle in the rotational direction in order to collect the spun filaments, and the spun filaments are spun by a smooth conveying wind. It has been proposed to transport them side by side in the axial direction.

However, since the passage defined by the "guide plate" has a constant vertical interval, the velocity of the conveying wind in the passage decreases toward the outer periphery.

Further, when the transport air is increased, a large amount of air near the rotary nozzle is sucked in depending on the flow velocity of the blowout air, and the surface of the rotary nozzle and the ambient temperature are lowered.

Further, turbulence easily occurs in the air flow in the passage, the spun fiber vibrates, and a large amount of air is required, resulting in waste of energy.

Japanese Unexamined Patent Publication (Kokai) No. 60-167908 proposes a device for conveying spun fibers composed of a pair of upper and lower "hollow rings" having an air inlet and an air discharge slit.

This pair of upper and lower "hollow rings" is disclosed in the above-mentioned Japanese Patent Laid-Open No. 59-
Similar to the "guide plate" of No. 150106, since it is provided in parallel in the vertical direction, the interval is constant.

For this reason, even in this device, it is inevitable that the velocity of the air decreases toward the outer periphery in the transfer passage defined by the pair of upper and lower “hollow rings”.

Further, when a large amount of air near the rotary nozzle is sucked in by the blowing of the transport air, the surface of the rotary nozzle and the ambient temperature are lowered.

In addition, this device, on the opposite surface of the "hollow ring",
A slit inclined toward the outer side in the radial direction of the rotary nozzle is provided, and by selecting the air pressure of the "hollow ring", the width and angle of the slit, the flight direction and speed of the spun fiber,
The strength can be changed arbitrarily.

However, also in this case, when the transport air is increased, a large amount of pressurized air is required and the air flow in the passage is easily disturbed.

(Problems to be Solved by the Invention) An object of the present invention is to prevent a decrease in temperature near a rotating nozzle and the occurrence of a necking phenomenon in a spinning process of a carbon fiber raw yarn to smoothly obtain a high-strength carbon fiber raw yarn. It is in manufacturing.

The inventors of the present invention have conducted experiments and studies repeatedly to keep the temperature near the rotating nozzle constant and control the air flow velocity so as to be uniform or accelerated from the nozzle opening to the outer peripheral direction thereof. We have found that air can prevent the necking phenomenon.

As a result of investigating the temperature distribution and the behavior of the air flow in the spinning process, the present invention has been completed.

(Means for Solving the Problems) The present invention relates to a centrifugal spinning device for pitch-based carbon fibers in which the rotation axis of the rotary nozzle is vertical and the discharge direction of the fibers is horizontal, and air is provided above and below the outer circumference of the rotary nozzle. The structure is such that a blow-out nozzle or slit is provided, and air blocking plates are provided above and below the outer circumference thereof, and the distance between the upper and lower air blocking plates becomes smaller toward the outer circumference.

Further, a space is provided between the air blowing nozzle or slit and the air blocking plate so that auxiliary air can flow in from the outside.

The flow velocity of the air blown from the air blowing nozzle or the slit into the spinning path defined by the upper and lower air blocking plates is uniform or accelerated toward the outer circumference.

(Operation) Regarding the point that the structure of the distance between the air blocking plates is made smaller toward the outer circumference, the present invention provides the air blocking plates above and below the outer circumference of the air blowing nozzle or the slit, and The distance is made smaller toward the outer circumference.

And, in the spinning path defined by the upper and lower air blocking plates, due to its structure, the flow velocity distribution of air is designed to be uniform or accelerated toward the outer periphery, so that the speed decrease or turbulence of the air Does not happen.

Therefore, when the centrifugal spinning device of the present invention is used, fibers immediately after spinning do not sag in the length direction, and thus fibers having a uniform yarn diameter, that is, a yarn without necking phenomenon can be spun.

Then, if this is further advanced to the infusibilizing step and the firing step, high-strength pitch-based carbon fibers can be manufactured.

This mechanism will be specifically described.

When there are air blowing nozzles or slits above and below the outer circumference of the rotary nozzle, and air blocking plates are provided above and below the outer circumference, and the intervals of the spinning paths defined by the upper and lower air blocking plates are parallel and constant. The cross-sectional area of the circumference of the opening of the spinning path increases as it goes toward the outer circumference.

Therefore, the flow velocity of air at an arbitrary point in the spinning path is r ₀ / R (r ₀ : outer radius of the air blowing nozzle or slit, R: radius of an arbitrary point through which air passes, and the spinning path is the above nozzle. Alternatively, since it is located on the outer circumference of the slit, the speed is always multiplied by the value of r ₀ <R.

For example, when a certain point on the spinning path is located at twice the radius of the air blowing nozzle or slit, the flow velocity of the air at that point is ½ of the flow velocity of the blowing air at the nozzle or slit. Becomes

Therefore, the fiber immediately after spinning ejected from the rotary nozzle is
A slack is generated in the middle of the spinning path, resulting in a fiber with a lot of necking.

On the other hand, in the case of the present invention, the distance between the spinning paths defined by the upper and lower air blocking plates becomes smaller toward the outer circumference, that is, the cross-sectional area of the circumference of the spinning path opening is equal at any point. Alternatively, it is configured such that the point located on the outer periphery is smaller.

For this reason, unlike the case where the interval is constant, the flow velocity of air in the spinning path is constant or accelerated, so that linear fiber without necking can be spun.

About a point where a space for inflowing auxiliary air is provided between the air blowing nozzle or slit and the air blocking plate. When air is blown into the spinning path from the air blowing nozzle or slit, a negative pressure is generated in the vicinity thereof. Then, since the negative pressure portion near the nozzle or the slit is compensated, the amount of air flowing in between the rotary nozzle and the air blowing nozzle or the slit increases.

For this reason, the surface of the rotary nozzle and the ambient temperature are lowered, and a spun yarn flying phenomenon occurs, or a necking phenomenon occurs in which the yarn diameter of the spun yarn is non-uniform in the length direction.

Further, when the temperature is extremely lowered, the nozzle port may be blocked by the spun yarn.

According to the present invention, since the auxiliary air is introduced from the outside with a space provided between the air blowing nozzle or the slit and the air blocking plate, this auxiliary air reduces the amount of air sucked in the vicinity of the rotary nozzle. , An ideal temperature distribution can be formed.

In particular, since the place where the space for inflowing the auxiliary air is provided is near the air blowing nozzle or the slit where the negative pressure is generated, this action becomes great.

(Example) The centrifugal spinning apparatus of the present invention relates to the spinning of pitch-based carbon fibers, but since it is particularly effective for spinning mesophase petroleum pitch, an example using this as a raw material will be described in detail below.

The present invention is not limited to this.

(Example 1) As shown in FIG. 1, a rotary nozzle 1 (radius: 100 mm,
Nozzle diameter: 0.3 mm x nozzle length: 1.2 mm, number of nozzle holes: 100 holes), inside diameter 210 above and below the outer circumference
mm, outside diameter 230 mm, air blowing nozzles 2 and 3 (nozzle hole number: 200 holes), and air above and below the outside, which has an inside diameter of 236 mm and an outside diameter of 390 mm, and whose cross-sectional view forms part of two hyperbolas. A pitch-based carbon fiber centrifugal spinning device including blocking plates 4 and 5 was used.

Using mesophase petroleum pitch with a softening temperature of 280 ° C as the raw material, the temperature of the rotating nozzle was controlled at 405 ° C, and the rotation speed was 4
Centrifugal spinning was carried out under conditions of 000 rpm and a flow rate of air from the air blowing nozzle of 55 m / s.

The obtained raw yarn was oxidized with air to make it infusible, and further carbonized at 1000 ° C. in a nitrogen atmosphere to produce carbon fiber.

When the strength of this carbon fiber was measured, it was 14.5 Ton / cm.
^{Was 2} .

(Example 2) As shown in FIG. 2, the rotary nozzle 1 (radius: 100 mm,
Nozzle diameter: 0.3 mm x nozzle length: 1.2 mm, number of nozzle holes: 100 holes), inside diameter 210 above and below the outer circumference
mm, outside diameter 230 mm, air blowing nozzles 2 and 3 (nozzle hole number: 200 holes), and above and below the outside, part of two straight lines with an inside diameter of 240 mm and an outside diameter of 390 mm, whose cross-sectional views are close to each other. A centrifugal spinning device for pitch-based carbon fibers composed of air blocking plates 4 and 5 to be formed was used.

Using mesophase petroleum pitch with a softening temperature of 270 ° C as the raw material, the temperature of the rotating nozzle was controlled at 390 ° C, and the rotation speed was 3
Centrifugal spinning was performed under the conditions of 800 rpm and a flow rate of air from the air blowing nozzle of 43 m / s.

The obtained raw yarn was oxidized with air to make it infusible, and further carbonized at 1000 ° C. in a nitrogen atmosphere to produce carbon fiber.

When the strength of this carbon fiber was measured, it was 14.1 Ton / cm.
^{Was 2} .

(Comparative Example 1) As shown in FIG. 3, the rotary nozzle 1 (radius: 100 mm,
Nozzle diameter: 0.3 mm x nozzle length: 1.2 mm, number of nozzle holes: 100 holes), inside diameter 210 above and below the outer circumference
mm, outside diameter 230 mm, air blowout nozzles 2 and 3 (nozzle hole number: 200 holes), and above and below that outside, form part of two straight lines with an inside diameter of 230 mm and outside diameter of 390 mm. Then, a pitch-based carbon fiber centrifugal spinning device consisting of punching plates 8 and 9 having a large number of holes was used.

Using mesophase petroleum pitch with a softening temperature of 280 ° C as the raw material, the temperature of the rotating nozzle was controlled at 405 ° C, and the rotation speed was 3
Centrifugal spinning was performed under the conditions of 800 rpm and a flow rate of air from the air blowing nozzle of 43 m / s.

The obtained raw yarn was oxidized with air to make it infusible, and further carbonized at 1000 ° C. in a nitrogen atmosphere to produce carbon fiber.

When the strength of this carbon fiber was measured, it was 9.0 Ton / cm ²
Met.

(Effect) The pitch-based carbon fiber centrifugal spinning apparatus of the present invention is configured such that the spacing between the spinning paths defined by the upper and lower air blocking plates becomes smaller toward the outer periphery, and the flow velocity of air in the spinning path becomes smaller. Characterized by constant speed or acceleration.

Therefore, the speed of the air blown into the spinning path from the air blowing nozzle or the slit in the spinning path does not decrease, and the linear fiber raw yarn without necking can be smoothly spun.

Further, according to the present invention, a space for inflowing auxiliary air from the outside is provided between the air blowing nozzle or slit and the air blocking plate.

For this reason, the amount of air sucked in near the rotary nozzle becomes small, the temperature of the rotary nozzle and the ambient temperature do not decrease, and a constant temperature distribution can be maintained, so that the necking phenomenon can be prevented from occurring and the spinning can be performed smoothly. .

As a result of the above, it is possible to smoothly produce high-quality carbon fibers having extremely high strength from the fiber raw yarn by the pitch-based carbon fiber centrifugal spinning device of the present invention.

According to the example of the present invention, the strength of the carbon fiber was 56 to 50, as compared with the comparative example in which the intervals of the punching plates were set in parallel.
Improved by 61%.

In addition, the present invention does not waste energy because it does not adopt the method of increasing the amount of air blown from the air blowing nozzle or slit as in the prior art in order to control the air velocity in the spinning path.

Furthermore, the present invention has a simple structure, so that it is easy to install,
It is economical.

[Brief description of drawings]

1 and 2 are cross-sectional views of the main parts of the centrifugal spinning device of the present invention. FIG. 3 is a main part sectional view of a conventional pitch-based carbon fiber centrifugal spinning apparatus. 1 ... Rotating nozzle 2 ... Air blow nozzle or slit (top) 3 ... Air blow nozzle or slit (bottom) 4 ... Air blocking plate (top) 5 ... Air blocking plate (bottom) 6 ... Straightening layer 7 ... Hyperbola 8 ... Punching plate (top) 9 ... Punching plate (bottom)

 ─────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP-A-60-167908 (JP, A) JP-A-59-150106 (JP, A) JP-A-60-199916 (JP, A) JP-B 47- 51966 (JP, B1)

Claims (1)

[Claims] 1. A pitch-based carbon fiber centrifugal spinning apparatus in which a rotary axis of a rotary nozzle is vertical and a fiber discharge direction is horizontal, and air blowing nozzles or slits are provided above and below the outer circumference of the rotary nozzle. Air blocking plates are provided above and below the outer circumference, and a space for injecting auxiliary air is further provided between the air blowing nozzle or slit and the air blocking plate, and the space between the upper and lower air blocking plates is reduced toward the outer circumference. A pitch-based carbon characterized in that the velocity of the air blown from the air blowing nozzle or slit into the spinning path defined by the upper and lower air blocking plates is uniform or accelerated toward the outer periphery. Fiber centrifugal spinning equipment.