Process for steam drawing carbon-fiber precursor acrylic fiber bundle

Abstract

This process for manufacturing a carbon-fiber precursor acrylic fiber bundle and this steam drawing apparatus are characterized in that the drawing of an acrylic fiber bundle with a pressured-steam drawing apparatus is conducted by: opening an acrylic fiber bundle by blowing a fluid thereto; supplying humidifying steam to the opened acrylic fiber bundle at a fiber temperature of 80 to 130 C. to adjust the water content of the fiber bundle to 3 to 7%; and thereafter drawing the resulting acrylic fiber bundle in a pressurized-steam atmosphere. Thus, the present invention can prevent the breaking of a single fiber, the fluffing of the fiber bundle, and the breaking of the whole of the fiber bundle, though such defects are susceptible to occurring in a case where an acrylic fiber bundle is drawn by steam drawing at a high draw ratio, at a higher speed, or into a fiber having a small denier.

Claims

1. A process for manufacturing a carbon-fiber precursor acrylic fiber bundle, comprising: drawing an acrylic fiber bundle in a pressurized steam atmosphere, and in the following order: opening the acrylic fiber bundle by spraying a fluid to the acrylic fiber bundle; preheating the opened acrylic fiber bundle to 80 C. to 130 C.; supplying a humidifying steam to the preheated acrylic fiber bundle thereby making the moisture content of the acrylic fiber bundle to be 3% to 7%; and drawing the humidified acrylic fiber bundle in a pressurized steam atmosphere.

2. The process according to claim 1, wherein the preheating is performed with a preheating roll or a heating plate.

3. The process according to claim 1, wherein the humidifying steam is supplied to the preheated acrylic fiber bundle by introducing the preheated acrylic fiber bundle into a yarn humidifying device to which the humidifying steam is supplied.

4. The process according to claim 1, wherein the humidifying steam is supplied to the preheated acrylic fiber bundle by spraying the humidifying steam to the preheated acrylic fiber bundle.

5. The process according to claim 1, wherein the humidifying steam supplied to the preheated acrylic fiber bundle is a saturated steam.

6. The process according to claim 1, comprising preheating the opened acrylic fiber bundle to 80 C. to 120 C.

7. The process according to claim 6, wherein the moisture content of the acrylic fiber bundle is made to be 4% to 6%.

8. The process according to claim 1, comprising preheating the opened acrylic fiber bundle to 80 C. to 100 C.

9. The process according to claim 8, wherein the moisture content of the acrylic fiber bundle is made to be 4% to 6%.

10. The process according to claim 9, comprising opening the acrylic fiber bundle by spraying air or steam to the acrylic fiber bundle at a flow rate of 300 to 700 NL/min and a pressure of 1 to 5 kgf/cm.sup.2.

11. The process according to claim 1, wherein the moisture content of the acrylic fiber bundle is made to be 4% to 6%.

12. The process according to claim 1, comprising opening the acrylic fiber bundle by spraying air or steam to the acrylic fiber bundle at a flow rate of 300 to 700 NL/min and a pressure of 1 to 5 kgf/cm.sup.2.

Description

BRIEF DESCRIPTION OF DRAWINGS

(1) FIG. 1 is a schematic cross-sectional view illustrating a steam drawing apparatus as a representative example of the present invention;

(2) FIG. 2 is a schematic cross-sectional view illustrating a steam drawing apparatus as a comparative example including a steam drawing device alone;

(3) FIG. 3 is a schematic cross-sectional view illustrating a steam drawing apparatus as a comparative example without an opening device and a preheating device;

(4) FIG. 4 is a schematic cross-sectional view illustrating a steam drawing apparatus as a comparative example without an opening device;

(5) FIG. 5 is a schematic cross-sectional view illustrating a steam drawing apparatus as a comparative example without a yarn humidifying device;

(6) FIG. 6 is a schematic cross-sectional view illustrating a steam drawing apparatus as a comparative example in which a preheating roll, an opening device, and a yarn humidifying device are disposed in this order;

(7) FIG. 7 is a schematic cross-sectional view illustrating a steam drawing apparatus as a comparative example in which a preheating roll, a yarn humidifying device, and an opening device are disposed in this order; and

(8) FIG. 8 is a schematic cross-sectional view illustrating a steam drawing apparatus as a comparative example in which a yarn humidifying device, a preheating roll, and an opening device are disposed in this order.

MODE(S) FOR CARRYING OUT THE INVENTION

(9) Hereinafter, the present invention will be described in detail. Before and after a pressurized steam drawing process, steps which are known in a fiber production field can be appropriately performed. For example, when an acrylic fiber is spun by a solution spinning method, the acrylic fiber is spun from a solution obtained by dissolving an acrylonitrile copolymer including co-monomer or an acrylonitrile homo-polymer as a raw material polymer in an well-known organic or inorganic solvent and is drawn by the steam drawing process of the present invention. In this case, the spinning method may be any one of a wet spinning, a dry/wet spinning, and a dry spinning, and as the subsequent steps, solvent removal, drawing in bath, oil agent application, drying, and the like can be performed. The steam drawing process may be performed in any step of the fiber production. As for the solution spinning, however, it is desirable to perform the steam drawing after a certain degree of solvent is removed from the fiber, that is to say, after the washing or the drawing in bath. Alternatively, it is desirable to perform the steam drawing after the drying. Here, the performing the steam drawing after the drying is more desirable from the viewpoint that a highly-oriented fiber is obtained.

(10) The steam pressure in which the drawing is performed is not particularly limited as long as the pressure is in a pressurized state and the pressure can be appropriately set to a pressure higher than the atmospheric pressure in accordance with the purpose. That is, the steam pressure is appropriately set in accordance with the type of the fiber to be drawn, the process state in the steam drawing step, or the targeted fiber properties.

(11) According to the present invention, it is important that the process for manufacturing a carbon-fiber precursor acrylic fiber bundle in which an acrylic fiber bundle is drawn in a pressurized steam atmosphere has a configuration wherein a fluid is sprayed to the acrylic fiber bundle so as to open the acrylic fiber bundle, humidifying steam is supplied to the acrylic fiber bundle of 80 C. to 130 C. so as to obtain a moisture content of 3% to 7% thereof, and the acrylic fiber bundle is drawn in a pressurized steam atmosphere.

(12) Accordingly, for example, even for the acrylic fiber bundle in which a plasticizing effect of steam is not easily obtained due to a water-repellent effect caused by silicone-based oil agent applied to the fiber, a plasticizing process is uniformly performed even inside the fiber bundle. Accordingly, even when the fiber bundle is drawn up to a high magnification in a steam drawing device, a fine fiber is to be produced, or a drawing speed is high, it is possible to prevent a trouble such as a breakage of the acrylic fiber bundle. Further, it is possible to prevent the breakage of the single filament or the fluff and hence to stably obtain the high-quality carbon-fiber precursor acrylic fiber bundle.

(13) It is desirable to open the acrylic fiber bundle with the opening device while spraying the fluid to the acrylic fiber bundle. The fluid used for opening the fiber bundle may be air, steam, water, organic solvent, or an inorganic or organic solution. Here, any one of these may be used as long as it does not cause a chemical reaction in the acrylic fiber bundle and gives an opening effect. However, air or steam is desirable in consideration of the workability in production. Generally, the opening process is performed by an opening nozzle, but if the traveling acrylic fiber bundle can be opened, the shape is not particularly limited. However, a nozzle capable of spraying a fluid in a direction perpendicular to the traveling acrylic fiber bundle can be desirably used. Further, when the fluid is air or steam, it is desirable that the flow rate be 300 to 700 NL/min and the pressure be about 1 to 5 kgf/cm.sup.2. By the opening process, the agglutination of the fibers with oil agent can be loosened. Thus, heat can be efficiently transferred from the steam in the subsequent steam drawing process.

(14) Further, the temperature of the acrylic fiber bundle that receives the humidifying steam after the opening process is desirably 80 C. to 130 C., more desirably 80 C. to 120 C., and further desirably 80 C. to 100 C. Thus, it is desirable to apply the humidifying steam to the acrylic fiber bundle at the temperature.

(15) When the temperature of the acrylic fiber bundle to be humidified is 80 C. to 130 C., the acrylic fiber bundle can efficiently obtain heat by condensation heat transfer caused by the steam.

(16) As for the acrylic fiber bundle, the fiber bundle temperature is high at the drying roll. For this reason, a preheating process is not necessary when the temperature of the acrylic fiber bundle immediately before the humidifying steam is applied thereto is 80 C. to 130 C. However, when the temperature is lower than 80 C., it is desirable to preheat the fiber bundle to 80 C. to 130 C. by using a preheating roll or a heating plate. It is desirable to perform the preheating process between the step (a) and the step (b).

(17) Subsequently, it is desirable to apply the humidifying steam to the fiber bundle immediately before the fiber bundle is introduced into the steam drawing device so that the moisture content of the acrylic fiber bundle is desirably 3% to 7% and more desirably 4% to 6%. When the moisture content is 3% to 7%, the plasticizing effect can be easily obtained. Further, as a method of applying the humidifying steam to the acrylic fiber bundle, it is desirable to use a method of passing the acrylic fiber bundle through the yarn humidifying device into which the humidifying steam is supplied or a method of spraying the humidifying steam to the acrylic fiber bundle. Further, it is desirable that the humidifying steam applied to the acrylic fiber bundle be saturated steam. Since the moisture content of the acrylic fiber bundle introduced into the steam drawing device is controlled, the plasticizing effect in the steam drawing device is more efficiently obtained, and hence the steam drawing process can be performed stably.

(18) Further, it is important that the steam drawing apparatus of the present invention has a configuration in which the opening device for opening the acrylic fiber bundle, the yarn humidifying device having a unit for supplying humidifying steam to the acrylic fiber bundle, and the steam drawing device which keeps an internal space in a pressurized state are disposed.

(19) Further, in order to preheat the acrylic fiber bundle, it is desirable to dispose a preheating roll or a heating plate having a unit for controlling a surface temperature between the opening device and the yarn humidifying device. Further, it is desirable to dispose the opening device between the drive rolls capable of controlling the tension of the acrylic fiber bundle. Further, it is desirable that in the steam drawing device a labyrinth seal portion is provided at each of the entrance and the exit of the drawing device through which the acrylic fiber bundle passes.

(20) By using the steam drawing apparatus, the efficient plasticizing effect is obtained. Even when the fiber bundle is drawn up to a high magnification, a fine fiber is to be obtained, or a drawing speed is high, it is possible to prevent a trouble such as a breakage of the acrylic fiber bundle. Further, it is possible to prevent the breakage of the single filament or the fluff and hence to stably obtain the high-quality carbon-fiber precursor acrylic fiber bundle.

EXAMPLES

(21) Hereinafter, the present invention will be described in more detail by referring to examples. Furthermore, in the example, the evaluation of the breakage of the entire carbon-fiber precursor acrylic fiber bundle was performed in a manner such that the steam drawing process was performed five times and the number of times of the breakage of the entire carbon-fiber precursor acrylic fiber bundle was counted.

(22) Further, the evaluation of the fluff of the carbon-fiber precursor acrylic fiber bundle was performed in a manner such that the traveling carbon-fiber precursor acrylic fiber bundle was observed by eyes for three minutes and the number of fluffs of the surface of the carbon-fiber precursor acrylic fiber bundle was counted. The breakage draw ratio was obtained by the following equation.
Winding Roll Speed (m/min)/Drawing Roll Speed (m/min)=Breakage Draw Ratio

Example 1

(23) Acrylic copolymer including acrylonitrile of 98 mol % and methacrylic acid of 2 mol % was dissolved into dimethylformamide so as to prepare a spinning dope of a polymer concentration of 23%. The spinning dope was ejected from a spinning nozzle into a coagulating bath at a temperature of 10 C. and a concentration of 80% so as to obtain a coagulated yarn. The coagulated yarn was drawn in cold water and then drawn in hot water, and was subjected to an oil agent application and a dry densification process so as to obtain an acrylic fiber bundle. Subsequently, the acrylic fiber bundle was drawn 4.0 times using a steam drawing apparatus 13 shown in FIG. 1 so as to obtain a carbon-fiber precursor acrylic fiber bundle in which the single filament fineness was 1.0 decitex and the number of filaments was 12000.

(24) In the steam drawing apparatus 13 shown in FIG. 1, the acrylic fiber bundle (the yarn) 1 is guided to the opening device 2 by a plurality of rolls. In the opening device 2, the fiber bundle is opened by the air blown in a direction perpendicular to the traveling acrylic fiber bundle 1 at the flow rate of 300 to 700 NL/min further desirably 400 to 500 NL/min.

(25) The acrylic fiber bundle 1 which is opened using the opening device 2 is preheated by the preheating roll 3, and is humidified with the yarn humidifying device 4 having a unit for supplying saturated steam.

(26) The acrylic fiber bundle 1 is preheated to 81 C. by the preheating roll 3, and is supplied to the yarn humidifying device 4.

(27) The saturated steam is supplied to the yarn humidifying device 4 through the steam supply pipe 5 and the condensed water is discharged from a drainage discharge port 6. The moisture content of the acrylic fiber bundle 1 is adjusted with the yarn humidifying device 4 to be 5.4%, and the acrylic fiber bundle 1 is supplied from the yarn humidifying device 4 to the steam drawing device 7.

(28) The steam drawing device 7 is formed so that the upper portion is covered by an upper lid 10 and the lower portion is covered by a stand 11, and the pressurized steam is supplied through a steam inlet 9. A labyrinth seal portion 8 is provided at each of the entrance and the exit of the acrylic fiber bundle 1, and the steam pressure inside the steam drawing device 7 is pressurized at 400 KPa. The carbon-fiber precursor acrylic fiber bundle is supplied from the steam drawing device 7 to a winding roll 12.

(29) A result for the evaluation of the number of times of breakage, the number of fluffs, and the breakage draw ratio of the obtained carbon-fiber precursor acrylic fiber bundle is shown in Table 1.

(30) TABLE-US-00001 TABLE 1 Temperature Moisture Number of of fiber content times of immediately of fiber cutting Yarn Steam before yarn after yarn acrylic Fluff Breakage Opening humidifying drawing Treatment order humidifying humidifying fiber (number/ Draw No. device Preheating roll device device {circle around (1)} is in upstream of process device ( C.) device (%) bundle 3 min) Ratio Figure Example 1 Provided Provided Provided Provided {circle around (1)} Opening {circle around (2)} Preheating {circle around (3)} Yarn {circle around (4)} Steam 81 5.4 0 0 8.0 1 device roll humidifying drawing device machine Example 2 Provided Provided Provided Provided {circle around (1)} Opening {circle around (2)} Preheating {circle around (3)} Yarn {circle around (4)} Steam 102 5.1 0 0 7.6 1 device roll humidifying drawing device machine Example 3 Provided Provided Provided Provided {circle around (1)} Opening {circle around (2)} Preheating {circle around (3)} Yarn {circle around (4)} Steam 129 5.2 0 0 7.0 1 device roll humidifying drawing device machine Example 4 Provided Provided Provided Provided {circle around (1)} Opening {circle around (2)} Preheating {circle around (3)} Yarn {circle around (4)} Steam 103 3.4 0 0 7.5 1 device roll humidifying drawing device machine Example 5 Provided Provided Provided Provided {circle around (1)} Opening {circle around (2)} Preheating {circle around (3)} Yarn {circle around (4)} Steam 101 7.1 0 0 7.4 1 device roll humidifying drawing device machine Comparative Not Not provided Not Provided {circle around (1)} Steam {circle around (2)} {circle around (3)} {circle around (4)} 27 5 21 4.0 2 Example 1 provided (used as provided drawing feeding roll) machine Comparative Not Not provided Provided Provided {circle around (1)} Yarn {circle around (2)} Steam {circle around (3)} {circle around (4)} 27 5.7 1 15 4.2 3 Example 2 provided (used as humidifying drawing feeding roll) device machine Comparative Not Provided Provided Provided {circle around (1)} Preheating {circle around (2)} Yarn {circle around (3)} Steam {circle around (4)} 101 5.2 1 10 4.5 4 Example 3 provided roll humidifying drawing device machine Comparative Provided Provided Not Provided {circle around (1)} Opening {circle around (2)} Preheating {circle around (3)} Steam {circle around (4)} 103 2 9 4.3 5 Example 4 provided device roll drawing machine Comparative Provided Provided Provided Provided {circle around (1)} Preheating {circle around (2)} Opening {circle around (3)} Yarn {circle around (4)} Steam 101 5.1 1 5 4.6 6 Example 5 roll device humidifying drawing device machine Comparative Provided Provided Provided Provided {circle around (1)} Preheating {circle around (2)} Yarn {circle around (3)} Opening {circle around (4)} Steam 101 4.9 3 14 4.0 7 Example 6 roll humidifying device drawing device machine Comparative Provided Provided Provided Provided {circle around (1)} Yarn {circle around (2)} Preheating {circle around (3)} Opening {circle around (4)} Steam 102 4.7 4 18 4.0 8 Example 7 humidifying roll device drawing device machine Values in Temperature of fiber immediately before yarn humidifying device of Comparative Examples 1, 4, and 7 are temperatures of fibers immediately before the steam drawing device.

Examples 2 to 5

(31) As shown in Table 1, the carbon-fiber precursor acrylic fiber bundle was obtained similarly to Example 1 except that the process condition of the steam drawing apparatus 13 was changed. A result for the evaluation of the number of times of breakage, the number of fluffs, and the breakage draw ratio of the obtained carbon-fiber precursor acrylic fiber bundle is shown in Table 1.

Comparative Example 1

(32) As shown in FIG. 2, the carbon-fiber precursor acrylic fiber bundle was obtained similarly to Example 1 except that a device other than the steam drawing device 7 was not provided. Furthermore, Reference Numeral 3 indicates a non-preheating feeding roll. A result for the evaluation of the number of times of breakage, the number of fluffs, and the breakage draw ratio of the obtained carbon-fiber precursor acrylic fiber bundle is shown in Table 1.

Comparative Example 2

(33) As shown in FIG. 3, the carbon-fiber precursor acrylic fiber bundle was obtained similarly to Example 1 except that the opening device 2 and the preheating roll 3 were not provided. Furthermore, Reference Numeral 3 indicates a non-preheating feeding roll. A result for the evaluation of the number of times of breakage, the number of fluffs, and the breakage draw ratio of the obtained carbon-fiber precursor acrylic fiber bundle is shown in Table 1.

Comparative Example 3

(34) As shown in FIG. 4, the carbon-fiber precursor acrylic fiber bundle was obtained similarly to Example 1 except that the opening device 2 was not provided. A result for the evaluation of the number of times of breakage, the number of fluffs, and the breakage draw ratio of the obtained carbon-fiber precursor acrylic fiber bundle is shown in Table 1.

Comparative Example 4

(35) As shown in FIG. 5, the carbon-fiber precursor acrylic fiber bundle was obtained similarly to Example 1 except that the yarn humidifying device 4 was not provided. A result for the evaluation of the number of times of breakage, the number of fluffs, and the breakage draw ratio of the obtained carbon-fiber precursor acrylic fiber bundle is shown in Table 1.

Comparative Examples 5 to 7

(36) As shown in FIGS. 6 to 8, the carbon-fiber precursor acrylic fiber bundle was obtained similarly to Example 1 except that the installation positions of the opening device 2, the preheating roll 3, and the yarn humidifying device 4 were changed. A result for the evaluation of the number of times of breakage, the number of fluffs, and the breakage draw ratio of the obtained carbon-fiber precursor acrylic fiber bundle is shown in Table 1.

EXPLANATIONS OF LETTERS OR NUMERALS

(37) 1: acrylic fiber bundle (yarn) 2: opening device 3: preheating roll 3: non-preheating feeding roll 4: yarn humidifying device 5: steam supply pipe 6: drainage discharge port 7: steam drawing device 8: labyrinth seal portion 9: steam inlet 10: upper lid 11: stand 12: winding roll 13: steam drawing apparatus