JPS6317123B2 - - Google Patents
Info
- Publication number
- JPS6317123B2 JPS6317123B2 JP10957281A JP10957281A JPS6317123B2 JP S6317123 B2 JPS6317123 B2 JP S6317123B2 JP 10957281 A JP10957281 A JP 10957281A JP 10957281 A JP10957281 A JP 10957281A JP S6317123 B2 JPS6317123 B2 JP S6317123B2
- Authority
- JP
- Japan
- Prior art keywords
- spinning
- nozzle
- holes
- diameter
- fineness
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 238000009987 spinning Methods 0.000 claims description 40
- 239000000835 fiber Substances 0.000 claims description 16
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 12
- 238000002166 wet spinning Methods 0.000 claims description 6
- 235000005074 zinc chloride Nutrition 0.000 claims description 6
- 239000011592 zinc chloride Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 4
- 229920002239 polyacrylonitrile Polymers 0.000 claims 1
- 230000015271 coagulation Effects 0.000 description 7
- 238000005345 coagulation Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 229920002972 Acrylic fiber Polymers 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920005594 polymer fiber Polymers 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Description
本発明は、繊度変動率の小さいアクリル系繊維
を得るための湿式紡糸用ノズルに関し、更に詳し
くは繊度変動率10％以下のアクリル系繊維を塩化
亜鉛系無機塩水溶液を使用して工業的規模で製造
するための湿式紡糸用ノズルに関するものであ
る。
繊度変動率を小さくすることは、紡糸時の工程
安定化や繊維性能の向上、更にアクリル系炭素繊
維の性能向上等に重要である。従来から原液過
の強化、ノズル洗浄の強化、紡糸浴整流化、吐出
単位の細分化等により、繊度変動率を小さくする
方法が提案されているが、従来の方法で繊度変動
率を10％以下にしようとすれば、特別な紡糸装置
や合糸のための設備等を用いねばならず、過大な
設備費が必要となつてくる。
特に塩化亜鉛系無機塩水溶液を溶媒とする紡糸
原液を凝固浴中に吐出する場合、塩化亜鉛の寄釈
熱によつて凝固時の温度が上昇し、繊度変動率を
大きくしている。すなわちこの希釈熱はノズル
（あるいは紡糸孔群）の外周においては、紡糸原
液が吐出された直後に多量の凝固液に接触するた
めに、殆んど温度の上昇がないが、ノズル中心部
においては凝固液の拡散が小さいために温度が上
昇する。
従つてノズル面の中心部と外周部では温度差よ
り紡糸原液の粘度に差を生じ吐出量の差異とな
る。
凝固時の温度差を小さくするには、ノズル面に
おいて紡糸孔の間隔（サークルピツチ及びステツ
プピツチ）を大きくしたり又はノズル面を適当に
分割して紡糸孔を配置したり、更に特別な凝固装
置を用いて、例えば１錘当りの紡糸孔数を100個
以下にして紡糸する方法、ノズル中央部より凝固
液を強制的に流出させる方法等を採用することが
考えられる。
しかしながら、上述の如き方法では繊度変動率
を15％以下にすることは難かしく、又特別な凝固
装置を用いた場合には過大な設備費が必要とな
る。
本発明は上述の如き欠点を解消し極めて簡単な
装置で繊度変動率を10％以下にできる湿式紡糸用
ノズルを提供せんとするものである。
ここに繊度変動率とは次式によつて計算された
ものである。
繊度変動率＝デニールの標準偏差／デニールの平均値
×100％
本発明の湿式紡糸用ノズルは、塩化亜鉛系無機
塩水溶液を使用してアクリロニトリル系重合体繊
維を製造するためのものであつて、ノズル全面に
おいて又はノズル全面を分割した各分割面におい
て、直径d1を有する紡糸孔が全孔数の10〜20％外
周部に、直径d3を有する紡糸孔が全孔数の２〜10
％中心部に、そして直径d2を有する紡糸孔が全孔
数の88〜70％残部にそれぞれ配置され、且つd1，
d2，d3の関係が下記式
0.60（d1）4≦（d2）4≦0.89（d1）4
1.1（d3）4≦（d2）4≦1.3（d3）4
を満足するものである。
本発明のノズルにあつては、全孔数の２〜10％
に当る紡糸孔を中心部に配置し、この紡糸孔の直
径d3を式の如く小さくすることにより、希釈熱
で粘度が低下して紡糸原液が過大に吐出すること
を防ぎ、他方全孔数の10〜20％に当る紡糸孔を外
周部に配置し、この紡糸孔の直径d1を式の如く
大きくすることにより、吐出量が過小になること
を防止して、もつて繊度変動率が10％以下になる
ように設計されている。直径d3を有する紡糸孔の
個数が全孔数の２％未満の場合には過大デニール
の繊維が生じ、10％を越える場合には過大デニー
ルは減少するものの過小デニールの繊維が増加す
る。
又直径d3に関し（1.1d3）4＞（d2）4の場合には過
大デニールの繊維を減少させる効果がなく、
（d2）4＞1.3（d3）4の場合には過小デニールの繊維が
増加する。
直径d1を有する紡糸孔の個数が全孔数の10％未
満の場合には過小デニール繊維が残り、20％を越
える場合には過大デニール繊維が生じたり、凝固
浴でのドラフト率が高くなりすぎて単糸切れを生
ずる。又直径d1に関し0.60（d1）4＞（d2）4の場合に
は過大デニールが増加し、（d2）4＞0.89（d1）4の場
合には過小デニールを減少させる効果がない。
従つてd1，d2，d3，の孔径及び孔数割合は、
各々全ての条件が満足されてはじめて繊度変動率
を10％以下にすることができるのである。
アクリル系重合体繊維紡糸用ノズルの直径は一
般には0.06〜0.18mmφ程度であり、本発明のノズ
ルにおいて残部に配置される紡糸孔の直径d2も通
常はこの程度のものである。この直径d2に基づき
直径d1及びd3は及び式から算出される。
以下本発明を第１〜３図によつて説明する。
第１図は紡糸用ノズル全面にべたに配列したも
のであり、外周に直径d1を中心に直径d3の紡糸孔
を有するノズルである。
第２，３図は紡糸孔を一定の紡糸孔群に分割し
たノズルであり、このような場合には各紡糸孔群
ごとにd1，d2，d3を有し、且つ一つの紡糸孔群が
100個以上の孔数であることが必要である。紡糸
孔群の孔数が100個以下で分割数の多い場合には、
そのノズルは第１図の如きべた配列と同様な取扱
いとなる。
本発明のノズルは上述の条件を満足するもので
あれば、この３種に限定されるものではなく、形
や紡糸孔群の数はいかなるものでもよい。
次に本発明を実施例により説明する。
実施例 １
塩化亜鉛48％と塩化ナトリウム10％とよりなる
混合塩水溶液を溶媒としてアクリロニトリル97
％、アクリル酸メチル３％の共重合体９％を含む
紡糸原液を調製した。この紡糸原液を第２図の如
きノズル、すなわち6000個の紡糸孔を15の紡糸孔
群に分割し、各群の最外周１重（d1）を0.069mm
φ、中心部（d3）を0.062mmφ、残部（d2）を
0.065mmφとして、各々の孔数割合はd1のもの16.5
％、d2のもの80％、d3のもの3.5％としたノズル
を用いて溶媒と同じ塩組成の10℃、30％水溶液中
に234ml／分の速度で吐出、凝固させ４ｍ／分で
引取つた。凝固された糸条は３倍の延伸をしなが
ら充分に水洗を行つた後、125℃の熱風で乾燥し、
次いで0.6Kg／cm2（ゲージ圧）の飽和水蒸気中で
4.5倍の延伸を行つた。
こうして得られた繊維は0.9デニール／フイラ
メント繊度変動率は7.8％と良好であつた。
比較例 １
各紡糸孔群の孔径をd1＝d2＝d3＝0.065mmφと
した以外は実施例１と同様に紡出した。
得られた繊維の平均繊度は0.9デニール／フイ
ラメントで繊度変動率は19.5％であつた。
実施例 ２
第１図の如く6000の紡糸孔がべた配列されたノ
ズルでd1＝0.069mmφ、d2＝0.065mmφ、d3＝0.062
mmφとし、各々の孔数割合の異なるノズルを用い
て実施例１と同様に紡糸し得られた繊維の繊度変
動率を測定し、第１表の結果を得た。
The present invention relates to a wet spinning nozzle for obtaining acrylic fibers with a small fluctuation rate of fineness, and more specifically, acrylic fibers with a fluctuation rate of fineness of 10% or less can be produced on an industrial scale using a zinc chloride-based inorganic salt aqueous solution. The present invention relates to a wet spinning nozzle for manufacturing. Reducing the variation in fineness is important for stabilizing the spinning process, improving fiber performance, and improving the performance of acrylic carbon fibers. Conventionally, methods have been proposed to reduce the fineness fluctuation rate by strengthening the raw solution filtration, strengthening the nozzle cleaning, rectifying the spinning bath, subdividing the discharge unit, etc., but conventional methods have not been able to reduce the fineness fluctuation rate to 10% or less. If this is attempted, special spinning equipment, equipment for doubling, etc. must be used, resulting in excessive equipment costs. In particular, when a spinning dope using an aqueous zinc chloride-based inorganic salt solution as a solvent is discharged into a coagulation bath, the temperature during coagulation increases due to the heat of the zinc chloride, increasing the fineness variation rate. In other words, this dilution heat causes almost no temperature rise at the outer periphery of the nozzle (or spinning hole group) because the spinning dope comes into contact with a large amount of coagulation liquid immediately after being discharged, but at the center of the nozzle, there is almost no rise in temperature. The temperature increases due to the small diffusion of the coagulating liquid. Therefore, the difference in temperature between the center and the outer periphery of the nozzle surface causes a difference in the viscosity of the spinning dope, resulting in a difference in the discharge amount. In order to reduce the temperature difference during coagulation, it is possible to increase the spacing between the spinning holes (circle pitch and step pitch) on the nozzle surface, to divide the nozzle surface appropriately and arrange the spinning holes, or to use a special coagulation device. It is conceivable to adopt, for example, a method in which the number of spinning holes per spindle is 100 or less, or a method in which the coagulated liquid is forcibly flowed out from the center of the nozzle. However, with the method described above, it is difficult to reduce the variation in fineness to 15% or less, and when a special coagulation device is used, excessive equipment costs are required. The present invention aims to eliminate the above-mentioned drawbacks and provide a wet spinning nozzle that can reduce the variation in fineness to 10% or less using an extremely simple device. Here, the fineness variation rate is calculated by the following formula. Fineness variation rate = Standard deviation of denier / Average value of denier × 100% The wet spinning nozzle of the present invention is for producing acrylonitrile-based polymer fiber using a zinc chloride-based inorganic salt aqueous solution, On the entire surface of the nozzle or on each dividing surface of the entire surface of the nozzle, spinning holes with a diameter of d 1 occupy 10 to 20% of the total number of holes, and spinning holes with a diameter of d 3 occupy 2 to 10 of the total number of holes.
% center, and spinning holes with a diameter d 2 are arranged in the remainder of 88-70% of the total number of holes, and d 1 ,
The relationship between d 2 and d 3 satisfies the following formula: 0.60 (d 1 ) 4 ≦ (d 2 ) 4 ≦0.89 (d 1 ) 4 1.1 (d 3 ) 4 ≦ (d 2 ) 4 ≦1.3 (d 3 ) 4 It is something to do. In the case of the nozzle of the present invention, 2 to 10% of the total number of holes
By arranging the spinning hole corresponding to By arranging spinning holes corresponding to 10 to 20% of It is designed to be less than 10%. If the number of spinning holes having a diameter d 3 is less than 2% of the total number of holes, over-denier fibers are produced, and if it exceeds 10%, over-denier fibers decrease but under-denier fibers increase. Also, regarding the diameter d 3 , if (1.1d 3 ) 4 > (d 2 ) 4 , there is no effect of reducing excessive denier fibers.
When (d 2 ) 4 > 1.3 (d 3 ) 4 , the number of underdenier fibers increases. If the number of spinning holes with a diameter d 1 is less than 10% of the total number of holes, undersized denier fibers will remain, and if it exceeds 20%, overly denier fibers will be produced or the draft rate in the coagulation bath will be high. Too much will cause single thread breakage. Regarding the diameter d 1, when 0.60 (d 1 ) 4 > (d 2 ) 4 , over-denier increases, and when (d 2 ) 4 > 0.89 (d 1 ) 4 , there is an effect of reducing under-denier. do not have. Therefore, the pore diameter and pore number ratio of d 1 , d 2 , d 3 are
Only when all conditions are satisfied can the fineness variation rate be reduced to 10% or less. The diameter of the acrylic polymer fiber spinning nozzle is generally about 0.06 to 0.18 mmφ, and the diameter d 2 of the spinning hole arranged in the remaining part of the nozzle of the present invention is also usually about this range. Based on this diameter d 2 , the diameters d 1 and d 3 are calculated from the following equations. The present invention will be explained below with reference to FIGS. 1 to 3. FIG. 1 shows a spinning nozzle that is arranged all over the surface, and has spinning holes with a diameter d 1 at the center and a diameter d 3 on the outer periphery. Figures 2 and 3 show a nozzle in which the spinning hole is divided into certain spinning hole groups, and in such a case, each spinning hole group has d 1 , d 2 , and d 3 , and one spinning hole is used. The group
The number of holes must be 100 or more. When the number of holes in the spinning hole group is 100 or less and the number of divisions is large,
The nozzles are handled in the same way as the solid arrangement shown in FIG. The nozzle of the present invention is not limited to these three types as long as it satisfies the above conditions, and any shape and number of spinning hole groups may be used. Next, the present invention will be explained by examples. Example 1 Acrylonitrile 97 was prepared using a mixed salt aqueous solution consisting of 48% zinc chloride and 10% sodium chloride as a solvent.
A spinning dope containing 9% of a copolymer of 3% and 3% of methyl acrylate was prepared. This spinning dope is divided into 15 spinning hole groups using a nozzle as shown in Figure 2, that is, 6000 spinning holes, and the outermost circumference (d 1 ) of each group is 0.069 mm.
φ, center part (d 3 ) is 0.062mmφ, remainder (d 2 ) is
Assuming 0.065mmφ, each hole number ratio is d 1 16.5
%, 80% of d2 and 3.5% of d3 were used to discharge into a 30% aqueous solution at 10℃ with the same salt composition as the solvent at a speed of 234 ml/min, solidify, and withdraw at 4 m/min. Ivy. The coagulated yarn was stretched 3 times and thoroughly washed with water, then dried with hot air at 125°C.
Then in saturated steam at 0.6Kg/cm 2 (gauge pressure)
It was stretched 4.5 times. The fiber thus obtained had a good filament fineness variation of 0.9 denier/filament fineness of 7.8%. Comparative Example 1 Spinning was carried out in the same manner as in Example 1 except that the diameter of each spinning hole group was set to d 1 = d 2 = d 3 = 0.065 mmφ. The average fineness of the obtained fibers was 0.9 denier/filament, and the fineness variation rate was 19.5%. Example 2 With a nozzle in which 6000 spinning holes are arranged in a uniform manner as shown in Fig. 1, d 1 = 0.069 mmφ, d 2 = 0.065 mmφ, d 3 = 0.062.
The fibers were spun in the same manner as in Example 1 using nozzles with different hole number ratios, and the fineness variation rate of the obtained fibers was measured, and the results shown in Table 1 were obtained.
【表】【table】
【表】
実施例 ３
3000の紡糸孔を有するベタ配列ノズルでd1，
d2，d3の各々の孔数割合を20％、75％、５％とし
て各孔径の異なるノズルを使用して実施例１と同
様に紡出した。得られた繊維の繊度変動率を測定
し、第２表の如き結果を得た。[Table] Example 3 With a solid array nozzle having 3000 spinning holes, d 1 ,
Spinning was carried out in the same manner as in Example 1 using nozzles with different hole diameters, with the hole number ratios of d 2 and d 3 being 20%, 75%, and 5%, respectively. The fineness variation rate of the obtained fibers was measured, and the results shown in Table 2 were obtained.
【表】
実施例 ４
d1，d2，d3を第３表の如く配分した第２図の如
きノズルを使用して実施例１に準じて紡出した。[Table] Example 4 Spinning was carried out according to Example 1 using a nozzle as shown in FIG. 2 in which d 1 , d 2 and d 3 were distributed as shown in Table 3.
【表】【table】
【表】
得られた繊維の平均繊度で0.90デニールで繊度
変動率は5.9％と良好であつた。[Table] The average fineness of the obtained fibers was 0.90 denier, and the fineness fluctuation rate was 5.9%, which was good.
第１〜３図は本発明の湿式紡糸用ノズルの１例
を示す概略図である。
1 to 3 are schematic diagrams showing one example of the wet spinning nozzle of the present invention.
Claims (1)
ニトリル系重合体繊維を製造するためのノズルで
あつて、ノズル全面において又はノズル全面を分
割した各分割面において、直径d1を有する紡糸孔
が全孔数の10〜20％外周部に、直径d3を有する紡
糸孔が全孔数の２〜10％中心部に、そして直径d2
を有する紡糸孔が全孔数の88〜70％残部にそれぞ
れ配置され、且つd1，d2，d3の関係が下記式 0.60（d1）4≦（d2）4≦0.89（d1）4 1.1（d3）4≦（d2）4≦1.3（d3）4 を満足するものである湿式紡糸用ノズル。[Scope of Claims] 1. A nozzle for producing acrylonitrile polymer fiber using a zinc chloride-based inorganic salt aqueous solution, which has a diameter d 1 on the entire surface of the nozzle or on each dividing surface of the entire surface of the nozzle. The spinning holes with a diameter of d 3 are located in the outer periphery, 2-10% of the total number of holes are located in the center, and the spinning holes with a diameter of d 2 are located in the center.
The spinning holes having 88 to 70% of the total number of holes are respectively arranged, and the relationship between d 1 , d 2 , and d 3 is expressed by the following formula: 0.60 (d 1 ) 4 ≦ (d 2 ) 4 ≦ 0.89 (d 1 ) 4 1.1 (d 3 ) 4 ≦ (d 2 ) 4 ≦ 1.3 (d 3 ) 4 A wet spinning nozzle that satisfies the following.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10957281A JPS5813714A (en) | 1981-07-14 | 1981-07-14 | Wet spinning nozzle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10957281A JPS5813714A (en) | 1981-07-14 | 1981-07-14 | Wet spinning nozzle |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5813714A JPS5813714A (en) | 1983-01-26 |
| JPS6317123B2 true JPS6317123B2 (en) | 1988-04-12 |
Family
ID=14513644
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10957281A Granted JPS5813714A (en) | 1981-07-14 | 1981-07-14 | Wet spinning nozzle |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5813714A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01209217A (en) * | 1988-02-17 | 1989-08-23 | Seiwa Seika Kk | Marshaling transport device for article |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0823083B2 (en) * | 1985-11-26 | 1996-03-06 | 日本エクスラン工業株式会社 | Acrylic fiber manufacturing method |
| JPS6342910A (en) * | 1986-08-07 | 1988-02-24 | Toho Rayon Co Ltd | Production of acrylonitrile yarn bundle for manufacturing carbon yarn |
| JPH0496502A (en) * | 1990-08-13 | 1992-03-27 | Nec Corp | Microwave monolithic integrated circuit |
| US20080095875A1 (en) * | 2006-10-10 | 2008-04-24 | Serge Rebouillat | Spinnerets for making cut-resistant yarns |
| US7638193B1 (en) * | 2006-10-10 | 2009-12-29 | E. I. Du Pont De Nemours And Company | Cut-resistant yarns and method of manufacture |
| JP5381130B2 (en) * | 2009-01-30 | 2014-01-08 | 東レ株式会社 | Wet spinning die and precursor fiber bundle for acrylic carbon fiber or method for producing carbon fiber |
| JP7352946B2 (en) * | 2019-09-05 | 2023-09-29 | ヤマシンフィルタ株式会社 | melt blowing equipment |
| JP7682016B2 (en) * | 2021-05-10 | 2025-05-23 | 帝人株式会社 | Spinning nozzle |
-
1981
- 1981-07-14 JP JP10957281A patent/JPS5813714A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01209217A (en) * | 1988-02-17 | 1989-08-23 | Seiwa Seika Kk | Marshaling transport device for article |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5813714A (en) | 1983-01-26 |
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