JP4827321B2

JP4827321B2 - Circular nozzle for wet spinning

Info

Publication number: JP4827321B2
Application number: JP2001160231A
Authority: JP
Inventors: 長徳和田; 信幸吉田
Original assignee: Toho Rayon Co Ltd
Current assignee: Toho Rayon Co Ltd
Priority date: 2001-05-29
Filing date: 2001-05-29
Publication date: 2011-11-30
Anticipated expiration: 2021-05-29
Also published as: JP2002348723A

Description

【０００１】
【発明の属する技術分野】
本発明は、湿式紡糸用円形ノズルに関し、更に詳述すればアクリロニトリル等の化学繊維を湿式紡糸法により製造する際に用いる円形ノズルに関する。
【０００２】
【従来の技術】
従来、アクリロニトリル等の化学繊維の紡糸方法として多数の吐出孔を形成したノズルを用いる湿式紡糸法がある。このノズルを用いる湿式紡糸法においては、同時に一個のノズルから多数の糸を紡糸することから、ノズル内の紡糸液温度の分布、凝固液の温度の分布、濃度の斑等に基因する繊維製品のデニール斑や凝固斑等が生じ易く、このため繊維製品の品質の変動が大きくなり易い。
【０００３】
これらの問題を解決するため、従来凝固液や紡糸液の整流化を行ったり、ノズルの吐出孔径に特定の分布を持たせること等が提案されている（特公昭６３−１７１２３号公報）。
【０００４】
また、円形ノズル面の吐出孔の穿孔領域を、中心及び所定半径の円から外方向に向う大小２種類の扇形に形成すると共に、各吐出孔から吐出される紡糸液量を調節することにより、上記問題を解決しようとする提案がある（特開平８−１３４７１２号公報）。
【０００５】
更に、ノズル表面における凝固液の流れを良好に保持するように、吐出孔の穿孔領域を亀甲のように配列した円形ノズルも提案されている。
【０００６】
また更に、３種類の孔径を有する吐出孔を所定の割合でノズル表面に配置したものも提案されている（特公昭６３−１７１２３号公報）。
【０００７】
これらの従来法によれば、ある程度の問題点の改善が認められている。しかし、デニール斑や凝固斑等を完全に抑制するには、未だ技術的に困難を伴うのが現状である。
【０００８】
【発明が解決しようとする課題】
本発明は上記事情に鑑みなされたもので、その目的とするところは、上記問題を解決した、デニール斑や凝固斑等の少ない高品位繊維製品を生産性良く製造することのできる、円形ノズルを提供することにある。
【０００９】
【課題を解決するための手段】
本発明者は、上記問題を解決するために種々検討した結果、扇形の吐出孔穿孔領域と、前記吐出孔穿孔領域間に所定幅で形成した凝固液流路形成用非穿孔領域を有する円形ノズルは、ノズル表面における凝固液の流入を円滑に行えること、及び前記形成した所定幅の非穿孔領域を流入する凝固液の冷却効果によりノズル内の吐出直前の紡糸液の冷却と、ノズル内紡糸液の有する温度斑とを相殺でき、その結果デニール斑や凝固斑等のない高品位繊維製品を製造できることを知得し、本発明を完成するに至った。
【００１０】
従って、上記目的を達成する本発明は以下に記載するものである。
【００１１】
〔１〕円形ノズルの円中心から外周にかけて形成された複数の略扇形穿孔領域と、前記複数の略扇形穿孔領域の間に形成された複数の非穿孔領域とからなる湿式紡糸用円形ノズルであって、前記扇形穿孔領域には円形ノズルの円中心を中心とする互いに等間隔離間する同心円上に所定間隔で穿設された吐出孔を有し、前記非穿孔領域は円形ノズルの外周から中心にかけて略同一幅に形成されてなることを特徴とする湿式紡糸用円形ノズル。
【００１２】
〔２〕同心円上に穿設された吐出孔数が２〜１９の穿孔領域においては、同心円上に穿設された吐出孔の両端吐出孔は扇形穿孔領域の両端直線上にあり、かつ非穿孔領域幅は最外周同心円上に穿設された吐出孔間距離の２〜４倍である〔１〕に記載の湿式紡糸用円形ノズル。
【００１３】
〔３〕最外周同心円上に穿設された吐出孔間距離が０．４５〜１．００ｍｍである〔２〕に記載の湿式紡糸用円形ノズル。
【００１４】
〔４〕吐出孔径が０．０４５〜０．１００ｍｍで、互いに隣接する同心円間距離が０．４〜０．９ｍｍである〔１〕乃至〔３〕の何れかに記載の湿式紡糸用円形ノズル。
【００１５】
【発明の実施の形態】
以下、図面を参照しながら本発明を詳細に説明する。
【００１６】
図１は、本発明湿式紡糸用円形ノズルのノズル面の一例を示すものである。図１中、１００はノズルで、円形のノズル面２には、円中心４を中心として外周６方向に向うに従って幅広になる複数の略扇形穿孔領域１０が均等に設けられている。そして、前記穿孔領域１０には、紡糸液の吐出孔（不図示）が複数穿設されている。
【００１７】
前記穿孔領域１０同士の間には、円中心４から外周６にかけて略同一幅の非穿孔領域１２が形成されている。
【００１８】
図２は、前記穿孔領域１０の部分拡大図で、互いに隣接する２つの穿孔領域３０、３２の間には円中心（不図示）からノズル外周（不図示）にかけて、略同一幅の非穿孔領域３４が形成されている。
【００１９】
穿孔領域の数としては、３０〜６０が好ましい。
【００２０】
穿孔領域３０、３２においては、円中心を中心とする等間隔の同心円３８上に紡糸液の吐出孔３６が穿設されると共に、同一同心円３８上の吐出孔３６は互いに等間隔に配列されている。そして、前記穿孔領域３０、３２は略扇形であるので、外周から円中心に向うに従い幅狭になり、これに伴い同心円上に形成される吐出孔の数は少なくなっている。このため、図１に示す円中心４から所定半径ｒ内の各穿孔領域１０は１つの同心円上に１個穿設された吐出孔により構成されることになる。なお、ｒは穿孔領域数、同心円間隔、穿孔間隔等により異なるが、通常ノズル面半径Ｒの５０％未満とされることが好ましい。
【００２１】
ノズルの半径Ｒは特に制限はないが、通常３０〜５０ｍｍが好ましい。
【００２２】
図２において、穿孔領域３２の各同心円３８上に穿孔された吐出孔３６が２以上の領域においては、同心円３８上に穿設された吐出孔３６のうち、両端の吐出孔３６ａ、３６ｂは扇形穿孔領域３２の両端の直線４０ａ、４０ｂ上にある。
【００２３】
吐出孔の孔径は紡糸液の種類、温度、粘度等により異なり特に制限がないが、通常０．０４５〜０．１ｍｍが好ましく、０．０５〜０．０８ｍｍがより好ましい。
【００２４】
吐出孔を穿設する同心円間の距離は上記同様特に制限がないが、０．４〜０．９ｍｍが好ましい。
【００２５】
同心円上の各吐出孔間の距離は、最外周同心円上に穿設された吐出孔の場合０．４５〜１．００ｍｍが好ましい。従って、同心円上の吐出孔の数が同一の場合は、円中心に向うに従って各吐出孔間距離は減少する。
【００２６】
各穿孔領域における最外周同心円上の吐出孔数は２０以下であることが好ましく、４〜１５が特に好ましい。
【００２７】
非穿孔領域３４の幅は、最外周同心円上に穿設された吐出孔間距離の２〜４倍が好ましい。
【００２８】
各穿孔領域、非穿孔領域は以上のように構成されている。
【００２９】
以下、実施例により本発明を更に具体的に説明する。
【００３０】
【実施例】
実施例１、２
表１に示す構成のノズルを作製し、湿式紡糸を行った。６０質量％の塩化亜鉛水溶液を溶媒として用い、これにアクリロニトリル９７質量％、アクリル酸メチル３質量％の共重合体（分子量８０００）を濃度７質量％に溶解させたものを紡糸原液として用いた。この紡糸原液を１０℃、２５質量％の塩化亜鉛水溶液中に吐出して凝固させた。
【００３１】
得られた凝固糸を１５〜９５℃の温水中で洗浄しながら合計３．２倍の多段延伸を行い、得られた繊維をアミノシリコンの水分散液（１０ｇ／ｌ）で処理した。その後、７０〜１５０℃のサクションドラム乾燥機で水分率が１質量％以下になるまで乾燥緻密化を行った。次いで、８０℃の熱水浴を通した後、０．７ｋｇ／ｃｍ²（ゲージ圧）の飽和水蒸気中で５倍の再延伸を行ってケンス内に振込み、０．９ｄｔｅｘ、１２０００本のストランドを得た。
【００３２】
このストランドをプレカーサーとして用いて、常法により２４０〜２７０℃の温度勾配を有する耐炎化炉で４０分間連続的に耐炎化処理を行い、次いで窒素気流中で３００〜１３００℃の温度勾配を有する炭素化炉で５分間炭素化処理して炭素繊維を得た。
【００３３】
融着数測定法
得られた長さ１００ｍの繊維束を１０ｍごとに長さ３ｍｍに切断して試料を得た。この試料をアセトン１０ｍｌに投入した後、超音波を１０秒間照射した。光学顕微鏡を用いて、倍率２０倍で前記繊維束を分散させたアセトン溶液を観察し、融着繊維の本数を数えた。
【００３４】
得られた結果を、表１に示した。
【００３５】
【表１】

【００３６】
比較例１、２
比較例１としてノズル面に均等に吐出孔を穿設したノズルを、比較例２として図３に示す吐出孔をノズル面に亀甲配列したノズルを用いる以外は実施例１と同様にして、表１に示す結果を得た。
【００３７】
【発明の効果】
本発明においては、上記のように構成したので、凝固液のノズル表面における流入を円滑に行え、形成した所定幅の非穿孔領域を流入する凝固液の冷却効果により、ノズル内の吐出直前の紡糸液の冷却と、ノズル内紡糸液の有する温度斑とを相殺でき、その結果デニール斑や凝固斑等のない高品位繊維製品を製造できる。
【図面の簡単な説明】
【図１】本発明ノズルの一例を示す一部省略平面図である。
【図２】図１のノズルの一部拡大平面図である。
【図３】比較例２で用いた亀甲ノズルを示す概略平面図である。
【符号の説明】
２ノズル面
４円中心
６外周
１０穿孔領域
１２非穿孔領域
３０、３２穿孔領域
３４非穿孔領域
３６吐出孔
３８同心円
３６ａ、３６ｂ両端の吐出孔
４０ａ、４０ｂ両端の直線
１００ノズル
Ｒノズルの半径[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a circular nozzle for wet spinning, and more particularly to a circular nozzle used when a chemical fiber such as acrylonitrile is produced by a wet spinning method.
[0002]
[Prior art]
Conventionally, there is a wet spinning method using a nozzle having a large number of discharge holes as a spinning method for chemical fibers such as acrylonitrile. In the wet spinning method using this nozzle, since a large number of yarns are spun from one nozzle at the same time, the spinning solution temperature distribution in the nozzle, the temperature distribution of the coagulation liquid, the density variation of the fiber products, etc. Denier spots, coagulation spots, and the like are likely to occur, and the fluctuations in the quality of the textile product are likely to increase.
[0003]
In order to solve these problems, it has been proposed to rectify the coagulating liquid and the spinning liquid and to give a specific distribution to the nozzle discharge hole diameter (Japanese Patent Publication No. 63-17123).
[0004]
In addition, by forming the perforated region of the discharge hole of the circular nozzle surface into two types of large and small sectors facing outward from the center and a circle with a predetermined radius, by adjusting the amount of spinning liquid discharged from each discharge hole, There is a proposal to solve the above problem (Japanese Patent Laid-Open No. 8-134712).
[0005]
Further, a circular nozzle in which the perforated areas of the discharge holes are arranged like a turtle shell has been proposed so that the flow of the coagulating liquid on the nozzle surface is well maintained.
[0006]
Furthermore, there has also been proposed one in which discharge holes having three types of hole diameters are arranged on the nozzle surface at a predetermined ratio (Japanese Patent Publication No. 63-17123).
[0007]
According to these conventional methods, some improvement of the problem is recognized. However, it is still technically difficult to completely suppress denier spots and coagulation spots.
[0008]
[Problems to be solved by the invention]
The present invention has been made in view of the above circumstances, and the object of the present invention is to provide a circular nozzle capable of producing a high-quality fiber product with reduced denier spots and coagulation spots with high productivity that solves the above problems. It is to provide.
[0009]
[Means for Solving the Problems]
As a result of various studies to solve the above problems, the present inventor has found that a circular nozzle having a fan-shaped discharge hole perforated region and a non-perforated region for forming a coagulating liquid channel formed with a predetermined width between the discharge hole perforated regions. Is capable of smoothly flowing the coagulating liquid on the nozzle surface and cooling the spinning liquid immediately before discharge in the nozzle by the cooling effect of the coagulating liquid flowing in the non-perforated region having the predetermined width, and the spinning liquid in the nozzle As a result, it was learned that a high-quality fiber product free from denier spots and coagulation spots could be produced, and the present invention was completed.
[0010]
Therefore, the present invention for achieving the above object is described below.
[0011]
[1] A circular nozzle for wet spinning comprising a plurality of substantially fan-shaped perforated regions formed from the circular center to the outer periphery of the circular nozzle, and a plurality of non-perforated regions formed between the plurality of substantially sector-shaped perforated regions. The fan-shaped perforated region has discharge holes perforated at predetermined intervals on concentric circles that are equally spaced apart from each other centered on the circular center of the circular nozzle, and the non-perforated region extends from the outer periphery to the center of the circular nozzle. A circular nozzle for wet spinning, characterized by being formed to have substantially the same width.
[0012]
[2] In the perforation region having 2 to 19 discharge holes drilled on the concentric circle, both end discharge holes of the discharge hole drilled on the concentric circle are on both straight lines of the fan-shaped perforation region and are not perforated The circular nozzle for wet spinning according to [1], wherein the region width is 2 to 4 times the distance between the discharge holes formed on the outermost concentric circle.
[0013]
[3] The circular nozzle for wet spinning according to [2], wherein the distance between the discharge holes formed on the outermost concentric circle is 0.45 to 1.00 mm.
[0014]
[4] The circular nozzle for wet spinning according to any one of [1] to [3], wherein the discharge hole diameter is 0.045 to 0.100 mm and the distance between adjacent concentric circles is 0.4 to 0.9 mm.
[0015]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, the present invention will be described in detail with reference to the drawings.
[0016]
FIG. 1 shows an example of the nozzle surface of a circular nozzle for wet spinning according to the present invention. In FIG. 1, reference numeral 100 denotes a nozzle, and the circular nozzle surface 2 is provided with a plurality of substantially fan-shaped perforated regions 10 that are widened in the direction of the outer periphery 6 with the circle center 4 as the center. In the perforated region 10, a plurality of spinning solution discharge holes (not shown) are formed.
[0017]
Between the perforated regions 10, a non-perforated region 12 having substantially the same width is formed from the circle center 4 to the outer periphery 6.
[0018]
FIG. 2 is a partially enlarged view of the perforated region 10, and a non-perforated region having substantially the same width from the center of a circle (not shown) to the outer periphery of the nozzle (not shown) between two adjacent

perforated regions

30 and 32. 34 is formed.
[0019]
The number of perforated areas is preferably 30-60.
[0020]
In the

perforated regions

30 and 32, the spinning solution discharge holes 36 are formed on concentric circles 38 that are equally spaced around the center of the circle, and the discharge holes 36 on the same concentric circle 38 are arranged at equal intervals. Yes. And since the said perforation area |

regions

30 and 32 are substantially fan-shaped, it becomes narrow as it goes to a circle center from an outer periphery, and the number of the discharge holes formed on a concentric circle is reduced in connection with this. For this reason, each perforation region 10 within a predetermined radius r from the circle center 4 shown in FIG. 1 is constituted by one ejection hole formed on one concentric circle. Note that r varies depending on the number of perforated regions, the distance between concentric circles, the distance between perforations, and the like.
[0021]
The radius R of the nozzle is not particularly limited, but is usually preferably 30 to 50 mm.
[0022]
In FIG. 2, in the region where two or more discharge holes 36 are formed on each concentric circle 38 in the perforated region 32, the

discharge holes

36a and 36b at both ends of the discharge holes 36 formed on the concentric circle 38 are fan-shaped. On the

straight lines

40a and 40b at both ends of the perforated region 32.
[0023]
The hole diameter of the discharge hole varies depending on the type of spinning solution, temperature, viscosity and the like and is not particularly limited, but is usually preferably 0.045 to 0.1 mm, and more preferably 0.05 to 0.08 mm.
[0024]
The distance between the concentric circles for forming the discharge holes is not particularly limited as described above, but is preferably 0.4 to 0.9 mm.
[0025]
The distance between the discharge holes on the concentric circle is preferably 0.45 to 1.00 mm in the case of the discharge holes drilled on the outermost concentric circle. Therefore, when the number of discharge holes on the concentric circle is the same, the distance between the discharge holes decreases toward the center of the circle.
[0026]
The number of discharge holes on the outermost concentric circle in each perforation region is preferably 20 or less, particularly preferably 4-15.
[0027]
The width of the non-perforated region 34 is preferably 2 to 4 times the distance between the discharge holes formed on the outermost concentric circle.
[0028]
Each perforated area and non-perforated area are configured as described above.
[0029]
Hereinafter, the present invention will be described more specifically with reference to examples.
[0030]
【Example】
Examples 1 and 2
Nozzles having the configuration shown in Table 1 were prepared and wet spinning was performed. A 60% by mass aqueous zinc chloride solution was used as a solvent, and a solution prepared by dissolving 97% by mass of acrylonitrile and 3% by mass of methyl acrylate (molecular weight 8000) at a concentration of 7% by mass was used as the spinning dope. This spinning dope was discharged into a 25% by mass zinc chloride aqueous solution at 10 ° C. and solidified.
[0031]
The obtained coagulated yarn was subjected to multistage drawing of 3.2 times in total while being washed in warm water at 15 to 95 ° C., and the obtained fiber was treated with an aqueous dispersion of aminosilicon (10 g / l). Thereafter, drying and densification were performed with a suction drum dryer at 70 to 150 ° C. until the moisture content became 1% by mass or less. Next, after passing through a hot water bath at 80 ° C., re-stretching is performed 5 times in saturated steam of 0.7 kg / cm ² (gauge pressure), and it is transferred into a can. 0.9 dtex, 12,000 strands are Obtained.
[0032]
Using this strand as a precursor, a flameproofing treatment is continuously carried out for 40 minutes in a flameproofing furnace having a temperature gradient of 240 to 270 ° C. by a conventional method, and then a carbon having a temperature gradient of 300 to 1300 ° C. in a nitrogen stream. Carbon fiber was obtained by carbonization for 5 minutes in a chemical furnace.
[0033]
Measurement method of fusion number A fiber bundle having a length of 100 m obtained was cut into a length of 3 mm every 10 m to obtain a sample. This sample was put into 10 ml of acetone and then irradiated with ultrasonic waves for 10 seconds. Using an optical microscope, an acetone solution in which the fiber bundle was dispersed at a magnification of 20 times was observed, and the number of fused fibers was counted.
[0034]
The obtained results are shown in Table 1.
[0035]
[Table 1]

[0036]
Comparative Examples 1 and 2
Table 1 shows the same as Example 1 except that a nozzle having discharge holes equally formed on the nozzle surface as Comparative Example 1 and a nozzle having the discharge holes shown in FIG. The result shown in was obtained.
[0037]
【The invention's effect】
In the present invention, since it is configured as described above, the spinning of the coagulating liquid on the nozzle surface can be smoothly performed, and the spinning immediately before the discharge in the nozzle can be performed by the cooling effect of the coagulating liquid flowing in the non-perforated region having a predetermined width. Cooling of the liquid and temperature spots of the spinning solution in the nozzle can be offset, and as a result, a high-quality fiber product free from denier spots and coagulation spots can be produced.
[Brief description of the drawings]
FIG. 1 is a partially omitted plan view showing an example of a nozzle of the present invention.
2 is a partially enlarged plan view of the nozzle of FIG. 1. FIG.
3 is a schematic plan view showing a turtle shell nozzle used in Comparative Example 2. FIG.
[Explanation of symbols]
2 Nozzle surface 4 Circle center 6 Peripheral area 10 Perforated area 12

Non-perforated area

30, 32 Perforated area 34 Non-perforated area 36 Discharge hole 38

Concentric circles

36a,

36b Discharge holes

40a, 40b Straight lines 100 at both ends Nozzle R Nozzle radius

Claims

A plurality of fan-shaped perforations area formed outwards from the circle center of the circular nozzle, a circular nozzle for wet spinning which consists of a plurality of non-perforated region formed between the plurality of fan-shaped perforations region,
The fan-shaped perforated region is subdivided into 30 to 60 by the non-perforated region,
Each of the fan-shaped perforated areas has discharge holes formed at predetermined intervals on concentric circles that are spaced apart from each other at equal intervals around the circle center of the circular nozzle,
The non-perforated region is formed to have the same width from the outer periphery to the center of the circular nozzle .
A circular nozzle for wet spinning.

The discharge holes are arranged on a concentric circle on the outer peripheral side of the circular nozzle so that the fan-shaped perforated region becomes narrower from the outer peripheral side toward the center of the circle, and on a plurality of concentric circles on the circular center side of the circular nozzle Then, one is formed on one concentric circle and arranged so as to form a straight line in the radial direction of the circular nozzle from the center of the circle.
The circular nozzle for wet spinning according to claim 1.

The discharge holes form a plurality of discharge hole group regions divided by the number of discharge holes drilled on one concentric circle,
The one area has a larger radial width than the other area adjacent to the area on the outer peripheral side of the circular nozzle.
The circular nozzle for wet spinning according to claim 1 or 2, characterized by the above.

In the perforated region having 2 to 19 discharge holes drilled on the concentric circle, the discharge holes at both ends of the discharge hole drilled on the concentric circle are on both straight lines of the fan-shaped perforated region, and the non-perforated region width is The circular nozzle for wet spinning according to any one of claims 1 to 3, wherein the nozzle is 2 to 4 times the distance between the discharge holes formed on the outermost concentric circle.

The circular nozzle for wet spinning according to claim 4 , wherein the distance between the discharge holes formed on the outermost concentric circle is 0.45 to 1.00 mm.

The circular nozzle for wet spinning according to any one of claims 1 to 5, wherein a discharge hole diameter is 0.045 to 0.100 mm, and a distance between adjacent concentric circles is 0.4 to 0.9 mm.